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Title:
PREPARATION OF N-ETHYLHYDROXYLAMINE HYDROCHLORIDE
Document Type and Number:
Japanese Patent JP2535711
Kind Code:
B2
Abstract:

PURPOSE: To safely prepare N-ethylhydroxylamine hydrochloride useful in the preparation of an intermediate of pharmaceuticals from di-t-butyl dicarbonate and hydroxylamine hydrochloride in a high yield and high purity.
CONSTITUTION: In the presence of an inert solvent, preferably water, dichloromethane or dioxane, in particular water and a base preferably selected from among Na2CO3, K2CO3, NaHCO3, NaOH, KOH and N(C2H5)3, 1 mol hydroxylamine hydrochloride is reacted with 2-3 mol di-t-butyl dicarbonate at 10-60°C for 0.5-6 hr to form N,O-bis-[1,1-dimethylethoxy]carbonyl]- hydroxylamine hydrochloride. This compd. is reacted with an ethylating agent, preferably an ethyl halide and the t-butyloxycarbonyl part of the ethylation product of formula III is cleaved with an acid to advantageously obtain the objective N-hydroxylamine hydrochloride of formula IV.


Inventors:
JOOJI II RII
Application Number:
JP25177892A
Publication Date:
September 18, 1996
Filing Date:
September 22, 1992
Export Citation:
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Assignee:
HOECHST ROUSSEL PHARMA (US)
International Classes:
C07C239/10; C07C239/08; C07C271/08; (IPC1-7): C07C239/08
Attorney, Agent or Firm:
Chika Takagi (2 outside)