CROSS-REFERENCE TO RELATED APPLICATIONS AND PRIORITY

The present application claims priority from Indian provisional patent application no. 202121005116 filed on the 05th day of February 2021, the details of which are incorporated herein by a reference.

TECHNICAL FIELD

The present subject matter described herein, in general, relates to a method of preparation of methoxyamine hydrochloride. In particular, the present subject matter is related to the preparation of high yield solid methoxyamine hydrochloride and a 30-40% solution of methoxyamine hydrochloride.

BACKGROUND

Methoxyamine hydrochloride (hereinafter alternatively referred as “MAHC1”) is a primary reagent used for preparation of one or more oxime derivatives. In state of the art, the conventional process of preparing MAHC1 lack in many aspects such as lower yield, loss of product, time consumption, low productivity and consumption of high amount of energy.

Therefore, there is a long felt need of developing an economic process for preparing Methoxyamine hydrochloride product by utilizing a different reaction route, minimizing the time consumption, and thereby minimizing the energy consumption of the overall process.

SUMMARY

This summary is provided to introduce concepts related to a preparation method of Methoxyamine hydrochloride (MAHC1). This summary is not intended to identify essential features of the claimed subject matter, nor it is intended for use in determining or limiting the scope of the disclosed subject matter.

In one embodiment, a process of preparing methoxyamine hydrochloride is disclosed herein. The process of preparation of Methoxyamine hydrochloride may comprise various stages and sub-steps implemented in a plurality of stages.

In one embodiment of the present invention, a first stage may include a preparation of hydroxylamine disulfonate (hereinafter alternatively referred as “HADS”). In a second stage, the process may comprise a step of methylation of HADS. In the third stage of the process, hydrolysis of methylated HADS is carried out to obtain Methoxyamine sulfate. In a fourth stage, the process may comprise Methoxyamine base recovery from the Methoxy amine sulfate in alkaline conditions. In a fifth stage, the process may involve conversion of Methoxy amine base to obtain Methoxy amine hydrochloride (MAHC1) by maintaining predetermined conditions. In a sixth stage, the process may comprise concentrating the crude reaction mass of Methoxyamine hydrochloride (MAHC1) to obtain a concentrated crude liquid mass of Methoxy amine hydrochloride (MAHCI). In a seventh stage, the process may comprise solidification and crystallization of the pre-determined amount of Methoxyamine hydrochloride (MAHCI) in a concentrated liquor form to obtain a final product of a solid Methoxy-amine hydrochloride (MAHCI).

List of Abbreviations

HADS- Hydroxylaminedisulfonic acid disodium salt

MADS- Methylhydroxylaminedisulfonic acid disodium salt

MAS- Methoxyamine sulfate

NODi - O,N-Dimethylhydroxylamine; N, O-Di methyl hydroxy laminc

MA Base - Methoxy amine Base

MAHCI - Methoxyamine Hydrochloride

DMS- Dimethyl sulfate

CSL- caustic soda lye (Sodium hydroxide)

DM water- Demineralized water

BRIEF DESCRIPTION OF FIGURES

The detailed description is described with reference to the accompanying Figures. In the Figures, the left-most digit(s) of a reference number identifies the Figure in which the reference number first appears. The same numbers are used throughout the drawings to refer like features and components.

Figure 1 depicts a method (100) of preparing a crude Methoxy amine hydrochloride in accordance with an embodiment of the present subject matter.

Figure 2 (a)-(f) depict a reaction assembly (200) for preparing a crude Methoxyamine hydrochloride in accordance with an embodiment of the present subject matter. Figure 2 (a) depicts a reaction tank (201, 202) of the reaction assembly (200) for preparation of alkaline HADS at stable alkaline pH in accordance with an embodiment of the present subject matter.

Figure 2 (b) depicts a reaction tank (203) of the reaction assembly (200) for Methylation of alkaline HADS in accordance with an embodiment of the present subject matter.

Figure 2 (c) depicts a reaction tank (204) of the reaction assembly (200) for alkaline distillation and Removal of O,N -Dimethylhydroxylamine; N, D-Di methyl hydroxy lamine (NODi) impurity from MADS liquor in accordance with an embodiment of the present subject matter.

Figure 2 (d) depicts a reaction tank (205) of the reaction assembly (200) for acid hydrolysis of MADS and acidic distillation in accordance with an embodiment of the present subject matter.

Figure 2 (e) depicts a reaction tank (206) of the reaction assembly (200) for Methoxyamine base recovery by using vacuum eductor pump in accordance with an embodiment of the present subject matter.

Figure 2 (f) depicts a reaction tank (207) of the reaction assembly (200) for obtaining Crude Methoxyamine hydrochloride in accordance with an embodiment of the present subject matter.

Figure 3 depicts a stage A of preparation (101) of alkaline Hydroxylamine disulfonic acid disodium salt (i.e., HADS) in accordance with an embodiment of the present subject matter.

Figure 4 depicts a stage B of methylation (102) of alkaline hydroxylamine disulfonate (HADS) to obtain the Methylhydroxylaminedisulfonic acid disodium salt liquor (MADS) in accordance with an embodiment of the present subject matter.

Figure 5 depicts a stage C of acid Hydrolysis (104) of MADS liquor to obtain acid hydrolyzed Methoxyamine sulfate (MAS) in accordance with an embodiment of the present subject matter.

Figure 6 depicts a stage D of methoxy amine base recovery (106) to obtain Methoxy amine base in accordance with an embodiment of the present subject matter. DETAILED DESCRIPTION

Reference throughout the specification to “various embodiments,” “some embodiments,” “one embodiment,” or “an embodiment” means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one embodiment. Thus, appearances of the phrases “in various embodiments,” “in some embodiments,” “in one embodiment,” or “in an embodiment” in places throughout the specification are not necessarily all referring to the same embodiment. Furthermore, the particular features, structures or characteristics may be combined in any suitable manner in one or more embodiments.

The words "comprising," "having," "containing," and "including," and other forms thereof, are intended to be equivalent in meaning and be open ended in that an item or items following any one of these words is not meant to be an exhaustive listing of such item or items or meant to be limited to only the listed item or items.

It must also be noted that, the singular forms "a," "an," and "the" include plural references unless the context clearly dictates otherwise. Although any methods similar or equivalent to those described herein can be used in the practice or testing of embodiments of the present disclosure, the exemplary methods are described. The disclosed embodiments are merely exemplary of the disclosure, which may be embodied in various forms.

Various modifications to the embodiment may be readily apparent to those skilled in the art and the generic principles herein may be applied to other embodiments. However, one of ordinary skill in the art may readily recognize that the present disclosure is not intended to be limited to the embodiments illustrated but is to be accorded the widest scope consistent with the principles and features described herein. The detailed description of the invention will be described hereinafter referring to accompanied drawings.

In one embodiment of the present invention, referring figure 1, a process (100) of preparing a crude Methoxyamine hydrochloride is illustrated in accordance with the embodiments of the present invention. The process (100) of preparation of Methoxyamine hydrochloride comprises of various steps and further divided into seven stages.

In one embodiment of the present invention, a first stage may include preparation of alkaline Hydroxyamine disulfonic acid disodium salt (i.e., HADS). In a second stage, the process (100) may include methylation of alkaline HADS to obtain Methylhydroxylaminedisulfonic acid disodium salt (MADS). In a third stage, acid hydrolysis of methylated HADS (MADS) may be carried out to obtain Methoxyamine sulfate. In a fourth stage, Methoxylamine base recovery may be performed in presence of caustic soda lye (NaOH) to remove the sulphate moiety and to obtain Methoxyamine. In a fifth stage, the process (100) may comprise obtaining crude Methoxy amine hydrochloride in presence of hydrochloric acid (HC1) to obtain Methoxyamine hydrochloride crude product (hereinafter alternatively referred as ‘Methoxyamine HC1’ ‘or ‘MAHC1’) by maintaining predetermined conditions. In a sixth stage, the process (100) may comprise concentrating the crude reaction mass of Methoxy amine hydrochloride (MAHC1) to obtain a concentrated crude liquid mass of Methoxy amine hydrochloride (MAHC1). In a seventh stage, the process (100) may comprise solidification and crystallization (109) of the pre-determined amount of Methoxy amine hydrochloride (MAHC1) in a concentrated liquor form to obtain a final product of a solid Methoxy-amine hydrochloride (MAHC1).

A first stage of Preparation (101) of alkaline HADS (Stage A)

In one embodiment of the present invention, the process (100) may include preparation (101) of alkaline Hydroxylamine di-sulfonic acid disodium salt (hereinafter may be alternatively referred as ‘HADS’) in stage (A). The HADS preparation (101) stage (A) may comprise an initial step of preparation of purified crystalline sodium nitrite (NaNCh). In one embodiment, improved form of purified crystalline sodium nitrite (NaNCh) with minimum impurities is obtained based on the disclosures of Indian Application No. 201921047080, filed on November 19, 2019, and titled “A venturi-air ammonia mixer enabled for two burner system”, and an Indian Application No. 201921004836, filed on 07 February 2019, and titled as “Apparatus and process for conversion of ammonia sodium nitrite” which are incorporated herein by a reference.

In one embodiment, in the first stage of Preparation (101) of HADS, external physicochemical conditions of a reactor assembly (200) are adjusted. In one embodiment, the adjusting of external conditions of the reactor assembly may include maintaining a cooling water pressure of a water hooter to not more than 1.5 kg/cm ² . In the next step, a heating steam temperature of the reactor assembly (200) is adjusted to not more than 2.0 kg/cm ² . In the next step, one or more reaction components may be fed into one or more reaction tanks of the reactor assembly (200).

Referring to figure 2 (a) and figure 3, preparation (101) of alkaline HADS (Stage A) is illustrated in accordance with an embodiment of the present invention. In one embodiment, a step of adding (301) one or more reactants such as a sodium nitrite (NaNCh) and caustic soda lye (NaOH) is performed, wherein the water may be fed to the overflow limit of the reaction tank (201) by pumping technique in order to obtain a premix of sodium nitrite (NaNCh) and caustic soda lye (NaOH). The ratio of the premix of sodium nitrite (NaNO2) and the caustic soda lye (NaOH) may be maintained as 1:1. In one embodiment, a concentration of caustic soda lye (NaOH) may be maintained between 47.3% to 49 % w/w. In one embodiment, a predetermined amount of Sulfur dioxide (SO2) gas may be fed to the reaction tank (201).

In one embodiment, the process of preparation (101) of alkaline HADS may further comprise a step of simultaneous mixing (302) of the premix of sodium nitrite (NaNO2) and the sodium hydroxide (NaOH) with feeding of SO2 gas to the reaction tank (201) for continuous preparation of acidic HADS. In one embodiment, the step of simultaneous mixing (302) of the premix of sodium nitrite (NaNO2) and sodium hydroxide (NaOH) with feeding of SO2 gas to the reaction tank (201) may be carried out in a circulatory motion by using a predetermined stirrer speed to obtain alkaline Hydroxylamine disulfonate (HADS) liquor in the reaction tank (201). In one embodiment, a huge power number for a small reactor (may be 3 kl) to the tune of 20-29 is maintained with a circulation rate of almost 30-50 times of the volume by enabling vigorous stirring. In one embodiment, the pH of a reaction mixture may be maintained between 2-5 and more preferably at a stable pH value of 2.8. In one embodiment, 12-18% of acidic HADS may be obtained.

In yet another embodiment, the acidic HADS having concentration of 12-18% w/v and a stable pH of 2.8-5 may be further transferred to a reaction tank (202) of a reactor assembly (200) by overflowing technique. In the reaction tank (202), a step of reacting (303) the acidic HADS with caustic lye (NaOH) may be performed to obtain the alkaline HADS. In one embodiment, a pH of the reaction tank (202) may be maintained at about 9-13 and preferably about 11. In one embodiment, the process of preparation (101) of the alkaline HADS is performed as a continuous process at a stable alkaline pH value of 9-12 and preferably 11. In one embodiment, the process implemented in stage (A) may lead to increase in an overall yield of alkaline HADS by at least 5%. The increase is felt by virtue of increase in water quantity to maintain the concentration as of before. In one example, water quantity is increased to 120 liter from 60 liter before. This is due to avoiding decomposition in the conventional batch process as compared to the continuous process.

A second stage of Methylation (102) of alkaline HADS to obtain MADS (Stage B) Referring to figure 1, in yet another embodiment of the present invention, the process (100) may comprise a second stage (B) of Methylation (102) of alkaline HADS to obtain the Methylhydroxylaminedisulfonic acid disodium salt (hereinafter may be alternatively referred as ‘methylated HADS’ or ‘MADS’).

Referring to figure 2 (a), 2 (b) of the reactor assembly (200) and figure 4, the second stage (B) methylation (102) of alkaline HADS to obtain MADS is illustrated in accordance with an embodiment of the present invention.

The second stage (B) of methylation (102) of alkaline HADS may also include charging (401) of alkaline HADS from reaction tank (202) into a reaction tank (203) of the reactor assembly (200). In one embodiment, the alkaline HADS may be fed to a reaction tank (203) through a gravitational filling technique in a continuous process.

In one embodiment of the present invention, the methylation (102) of alkaline HADS may further include a step of heating (402) of alkaline HADS to a temperature range of 60 °C-80 °C, preferably between a temperature range of 65 °C-72°C, and more preferably at 70°C in the reaction tank (203). In one embodiment, the step of heating is carried out with the help of a steam jacket heating technique.

In one embodiment of the present invention, the methylation (102) of alkaline HADS may further include a step of maintaining (403) a predetermined pH level by mixing of caustic soda lye (NaOH) inputted from a reservior with the alkaline HADS in the reaction tank (203). In one embodiment, the pH level may be maintained between 9-12.

In one embodiment, the reaction tank (203) may work as an agitation tank (203), wherein while inputting the caustic soda lye (NaOH) into the reaction tank (203) comprising alkaline HADS, the agitation tank (203) may be kept in circulatory motion for the proper mixing with the caustic soda lye (NaOH). In one embodiment the time period for mixing of one or more components in the reaction tank (203) may be maintained between 30 minutes to 2 hours and preferably 1 hour.

In one embodiment of the present invention, the step of methylation (102) may comprise a step of reacting (404) by continuous addition of di-methyl sulfate (DMS) (95.0 to 99.0 % w/w) from a reservoir with the premix of caustic soda lye (NaOH) and alkaline HADS having a predetermined alkaline pH level (as described above) in the reaction tank (203) at a predetermined time period of 4 to 6 hours as per batch size and temperature ranging between 62 °C -75 °C). In one embodiment, continuous addition of accurate quantity of dimethyl sulfate (DMS) in 0.80 ± 1 mole ratio to the agitation tank (203) may be performed at stage B or in step of methylation (102) of alkaline HADS. Here, the yield improvement of MADS along with time reduction to the tune of 1 hour and thereby reducing maintenance time is reduced from 5 hours to 4 hours) is achieved by making the process semi-continuous via-a-vis lot wise addition in the conventional art.

In yet another embodiment, while charging the di-methyl sulfate (DMS) to the reaction tank (203), a temperature of reaction tank (203) may be maintained at about 72+10 °C and more preferably between 65°C-68 °C by adjusting heating and cooling jerk mechanism of the steam jacket before charging of caustic soda lye (NaOH) to the reaction tank. The heating and cooling jerk mechanism is implemented by simultaneous operations of heating and cooling cycles to maintain the temperature. In one embodiment, the time period for reacting of di-methyl sulfate (DMS) 95.0 to 99.0 % with the premix of caustic soda lye (NaOH) and alkaline HADS may be adjusted between 2-5 hours and preferably about 2.5 hours.

In yet another embodiment, optionally, another batch of caustic soda lye (NaOH) to the reaction tank (203) may be charged for maintaining the alkaline pH of a reaction mixture comprising alkaline HADS, di-methyl sulfate (DMS) and caustic soda lye (NaOH) to obtain a higher yield of methylated HADS.

In one embodiment, the charging of the predetermined amount of caustic soda lye (NaOH) and the predetermined amount of Dimethyl sulfate (DMS) (which is as per the mole ratio of 0.8:0.9 moles of DMS based on Sodium Nitrite added) may be carried out by way of continuous addition of both the components comprising caustic soda lye (NaOH) and Dimethyl sulfate (DMS) to achieve a stable alkaline pH level of 10.5 and to obtain an improved yield of methylated HADS i.e., Methylhydroxylaminedisulfonic acid disodium salt (MADS) liquor. In yet another embodiment, the simultaneous and continuous addition of caustic soda lye (NaOH) and Dimethyl sulfate (DMS) may lead to reduction in overall digestion time of a reaction mixture upto 2.5-4 hours.

In one embodiment, the Methylhydroxylaminedisulfonic acid disodium salt (hereinafter may be alternatively referred as ‘MADS’) liquor may comprise an amount of free alkaline component i.e., caustic soda lye (NaOH). In one embodiment, the % free alkaline substance is about 0.5% to 4%. The MADS liquor comprising a minor amount of free alkaline component may be further transferred to a reaction tank (204) for performing a third stage of Hydrolysis of (MADS) liquor to obtain acid hydrolyzed Methoxyamine sulfate (hereinafter may be alternatively referred as ‘MAS’).

A third stage of acid hydrolysis (104) of MADS liquor to obtain acid hydrolyzed Methoxyamine sulfate (MAS) C) In still another embodiment of the present invention, the process (100) may comprise a third stage (C) of acid Hydrolysis (104) of MADS liquor to obtain acid hydrolyzed Methoxyamine sulfate (MAS).

Referring to Figure 2 (b), 2 (c) and 2 (d) of the reactor assembly (200) and figure 5, the third stage (C) of acid hydrolysis of MADS liquor to obtain acid hydrolyzed MAS is illustrated in accordance with an embodiment of the present invention.

The third stage C of acid hydrolysis (104) of MADS liquor may include transferring (501) of MADS liquor comprising a predetermined amount of free alkaline component from the reaction tank (203) into a reaction tank (204) of the reactor assembly (200). In one embodiment, transferring (501) of the MADS liquor to the reaction tank (204) may be performed by gravitational feeding technique for the acid hydrolysis and conversion of MADS liquor to acid hydrolyzed Methoxyamine sulfate (MAS).

In yet another embodiment, optionally, excess amount of caustic soda lye (NaOH) may be added to the reaction tank (204) for maintaining the alkaline pH and free-alkaline component content of a reaction mixture comprising MADS liquor. In still another embodiment, the content of free alkaline content (free NaOH) of the MADS liquor may be maintained at about 1.3% for efficient completion of the alkaline distillation and overall acid hydrolysis process in alkaline conditions and for reduction in, N-Dimethylhydroxylamine, N,0 -Dimethylhydroxylamine (NODi) impurity formed at stage 3.

In one embodiment, when the free alkaline % of the MADS liquor is observed to be less than 1.3%, then optionally, an additional amount of caustic soda lye (NaOH) is added intermittently to the reaction tank (204).

Alkaline distillation

Referring to Figure 2(c), in one embodiment of the present invention, the method (100) may comprise a step of alkaline distillation of the MADS liquor for recovery (105) of alkaline water at the temperature range of 100°C - 113°C. In one embodiment, in the step of alkaline distillation, the reaction mass between the temperature range of 100°C - 113 °C is performed by a steam jacket heating technique.

In another embodiment of the present invention, the method (100) may comprise a step of recovery (105) of alkaline water from the MADS liquor by using two or more heat exchangers to remove the alkaline water and unknown impurities such as O,N -Dimethylhydroxylamine; N,O- Dimethylhydroxylamine (NODi) impurity from the reaction tank (204) and to obtain impurity free MADS. In one embodiment the alkaline water is further transferred to an effluent treatment plant for further purification process as per the standard effluent treatment guidelines.

In one embodiment, the reduction in water distillation quantity by at least 60-65% is achieved at the step of recovery of alkaline water by alkaline distillation of MADS liquor by using a continuous process as described in the Stage A and the Stage B. In one embodiment, the impurity free MADS is transferred to the reaction tank (205) for the acidic distillation of MADS and to obtain the Methoxyamine sulfate (MAS) product. In this step, the improvement is achieved by doing negative experiments with respect to required water removal and establishing right quantity which is at least 60-65% lesser resulted in time cycle reduction to the tune of 3-4 hours. In an example, the withdrawal quantity of alkaline water may be varied from 0 to maximum level to obtain the benchmark figure of 240kg reduced from 900kg by calculating end to end results.

Acidic distillation

Referring to Figure 2(d), in one embodiment of the present invention, the method (100) may comprise a step of cooling (502) of the impurity free MADS to a temperature range of 55°C -60°C in the reaction tank (205). In one embodiment, cooling (502) of the impurity free MADS from 113 °C to the temperature at about 55°C -60°C may be carried out by using steam water jacket cooling.

In one embodiment, when the reaction mass is cooled down to the predetermined range of 55°C - 60°C, a step of slow addition (503) of H2SO4 for adjusting a predetermined acidic pH may be performed.

In the next step, acid distillation (504) of the impurity free MADS to obtain Methoxyamine sulfate (MAS) may be performed. In one embodiment of the present invention, the method (100) may comprise a step of acid distillation (504) by gradual increment in the temperature to reach out to a total reflux condition and to obtain Methoxy amine sulfate (MAS) product. In one embodiment, a pH of the reaction mass comprising MADS and cone. H2SO4 is maintained as highly acidic, that is at the level of pH 2-6 to carry out the acid hydrolysis. In one embodiment, gradual increment in temperature is achieved by heating the reaction mass comprising MADS and cone. H2SO4 gradually up to 113°C to reach on total reflux condition for the time period of one hour to obtain Methoxyamine sulfate (MAS). In one embodiment, recovery (105) of acidic water from the reaction mass may be performed by using acid reflux methodology and the acidic water may be further transferred to an effluent treatment plant for further purification process as per the standard effluent treatment guidelines. In one embodiment, the Methoxyamine sulfate (MAS) may be further transferred to the reaction tank (206) for basification of MAS and to obtain Methoxyamine base product.

A fourth stage of Methoxyamine base recovery 106) to obtain Methoxyamine base (Stage D) (106) to obtain Methoxyamine base (Stage D)

In yet another embodiment of the present invention, the process (100) may comprise a fourth stage of Methoxyamine base recovery (106) in presence of caustic soda lye (NaOH) to remove the sulphate moiety and to obtain Methoxyamine base (hereinafter may be alternatively referred as ‘Methoxyamine base’ or ‘MA base’)

Referring to Figure 2(e) of the reactor assembly (200) and figure 6, the fourth stage of methoxyamine base recovery (106) of Methoxyamine sulfate (MAS) to obtain Methoxyamine base may be performed in a reaction tank (206).

In one embodiment of the present invention, the fourth stage of methoxyamine base recovery (106) of Methoxyamine sulfate (MAS) may be performed at the cooling temperature of 40°C - 45 °C by addition (602) of the caustic soda lye (NaOH) from the reservior. In one embodiment, the addition (602) of the caustic soda lye (NaOH) to the reaction tank (206) comprising Methoxyamine sulfate (MAS) may be performed by partial addition technique.

In one embodiment the reaction tank (206) may be an eductor reactor. In this process, the atmospheric distillation of the active ingredient (MAB) is converted to vacuum distillation using special material (like PTFE, PFA, ETPFA, PVRC, special PP etc.) of construction of eductor suitable for the highly corrosive environment resulted in reducing the losses of the active ingredient (MAB) which is having very low boiling point of less than 50 degree C. The eductor system is a combination of an eductor with design intent of creating required vacuum to take the active ingredient gases (MAB) and mix them with the circulating HC1 solution by giving the effect of 4-5 m packed column. The eductor reactor (206) may be configured to perform basification reaction and methylamine base (MAB) distillation. In one embodiment, at this stage, the pH level of the reaction mass comprising Methoxylamine base may be maintained between 7-9. In another embodiment, the step of basification may comprise cooling down (601) of the reaction mass comprising of Methoxyamine sulfate to a temperature between 40°C-45°C and then a predetermined amount of caustic soda lye (NaOH) maybe gradually added to the reaction mixture to obtain the Methoxy amine base intermediate product. At this point temperature of the reaction mass is maintained preferably below 60°C.

In one embodiment, the reaction tank (206) may comprise a vacuum eductor pump configured for the recovery of Methoxy amine base. In one embodiment, the vacuum range of the vacuum eductor pump is maintained in the range of 630-670 mmHg. In one embodiment, vacuum should be maintained at the variation ± 5%. In one embodiment, the operating conditions of the vacuum eductor pump may be maintained such that the pump discharge pressure is maintained between 2.5 to 3.5 Kg/cm ² and the vacuum range is maintained between (630-670 mmHg.), vacuum eductor pump at about 700 mmHg.

A fifth stage of acidification (107) of Methoxylamine base and obtaining Crude Methoxylamine hydrochloride (Stage E)

In yet another embodiment of the present invention, the process (100) may comprise a fifth stage of obtaining Crude Methoxylamine hydrochloride (E) in presence of hydrochloric acid (HCL) to obtain Methoxylamine hydrochloride crude product. (Hereinafter alternatively referred as ‘Methoxylamine.HCr or ‘MAHC1’). Further, obtaining of Crude Methoxylamine hydrochloride is performed in a reaction tank (207) in accordance with the embodiment of the present invention.

In one embodiment, a step of recovery (106) of methoxy amine base from an eductor reactor (206) using a vacuum eductor pump may be performed. The methoxy amine base recovered from the educator reactor (206) may be further transferred to a reaction tank (207) comprising hydrochloric acid (HC1) for reacting with hydrochloric acid (HC1) and to synthesize a Crude Methoxylamine hydrochloride (MAHC1) product.

Referring to Figure 2(f) of the reactor assembly (200), addition of predetermined amount of HC1 in the reaction tank (207) may be carried out. In one embodiment, at this stage addition of a reaction mass of Methoxylamine base to the reaction tank (207) comprising HC1 may be performed. The pH level of the reaction mass comprising Methoxy amine base and HC1 maybe maintained between 8.3- 8.5. In another embodiment, the temperature of the Methoxyamine base may be cooled down to 20 to 25 °C by applying chilling water jacket technique.

In one embodiment of the present invention, a step of acidification (107) of Methoxyamine base performed by reacting Methoxyamine base with concentrated HC1 at the temperature of 20 to 25 °C in reaction tank (207) to obtain crude Methoxy amine hydrochloride.

In one embodiment, additionally a predetermined amount of cold HC1 having temperature between 25°C-20°C may be added to the reaction mixture comprising Methoxyamine base to obtain desired product of crude Methoxy amine hydrochloride (MAHC1).

A sixth stage of concentrating (108) the crude reaction mass of Methoxyamine hydrochloride (MAHC1) to obtain a concentrated crude liquid mass of Methoxyamine hydrochloride (MAHC1) (Stage F)

In one embodiment of the present invention, a stage (F) of concentrating (108) the crude reaction mass of Methoxyamine hydrochloride (MAHC1) may be carried out in the reaction tank (207) to obtain a concentrated crude liquid mass of Methoxy amine hydrochloride (MAHC1) by recovery of Methoxyamine base.

In another embodiment, of the present invention, a method of obtaining a solid and liquid concentrated form of Methoxyamine hydrochloride (MAHC1) is disclosed. In the first step, heating of the crude Methoxyamine hydrochloride (MAHC1) liquid to the temperature range of 55°C-60°C may be carried out by Reboiler for evaporation of excess amount of liquid content from the crude liquid mass of Methoxyamine hydrochloride (MAHC1) and to obtain 30-40% solution of methoxyamine hydrochloride, (MAHC1) ) in a concentrated liquor form.

A seventh stage of solidification and crystallization (109) of the pre-determined amount of Methoxyamine hydrochloride (MAHC1) in a concentrated liquor form to obtain a final product of a solid Methoxy-amine hydrochloride (MAHC1) (Stage G)

In the next optional stage (G), solidification and crystallization (109) of the pre-determined amount of Methoxyamine hydrochloride (MAHC1) in a concentrated liquor form may be carried out to obtain a final product of a solid Methoxy-amine hydrochloride (MAHC1). In an alternate embodiment Methoxylamine Hydrochloride solid is obtained in stage G of solidification and crystallization (109) of the Methoxyamine hydrochloride (MAHC1).

In another embodiment of the present disclosure the Methoxyamine Hydrochloride (MAHCL) obtained in accordance with the present invention may be a white or yellowish crystal, easily soluble in water, soluble in ethanol.

In another embodiment of the present disclosure the Methoxyamine Hydrochloride (MAHCL) obtained in accordance with the present invention may be used for producing the antibiotic medicines and bactericide such as the Cefuroxime Acid.

In accordance with embodiment of the present disclosure, a process of preparing Methoxyamine hydrochloride (MAHC1) described above have following advantages including but not limited to:

• Increment in final yield of Methoxyamine hydrochloride (MAHC1) up to 49-50%.

• Minimizing requirement of removal of amount of alkaline water at the step of alkaline distillation.

• Reduction in time and energy consumption of the overall process of obtaining Methoxyamine hydrochloride (MAHC1).

The instant invention is further described by the following experimental section:

The embodiments, examples and alternatives of the preceding paragraphs or the description and drawings, including any of their various aspects or respective individual features, may be taken independently or in any combination. Features described in connection with one embodiment are applicable to all embodiments, unless such features are incompatible.