METHOD FOR PURIFYING 1-(4-AMINO-2-METHYLBENZOYL)-7-CHLORO-5-OXO-2,3,4,5-TETRAHYDRO-1H-1-BENZAZEPINE

Title:

METHOD FOR PURIFYING 1-(4-AMINO-2-METHYLBENZOYL)-7-CHLORO-5-OXO-2,3,4,5-TETRAHYDRO-1H-1-BENZAZEPINE

Document Type and Number:

Japanese Patent JP2018024637

Kind Code:

A

Abstract:

PROBLEM TO BE SOLVED: To provide a method for purifying 1-(4-amino-2-methylbenzoyl)-7-chloro-5-oxo-2,3,4,5-tetrahydro-1H-1-benzazepine, which is one of the producing intermediates of tolvaptan.SOLUTION: This invention relates to a purification method, comprising the steps of: (a) making a rough 1-(4-amino-2-methylbenzoyl)-7-chloro-5-oxo-2,3,4,5-tetrahydro-1H-1-benzazepine react with sulfonic acid, to conduct isolation as a sulfonate; (b) recrystallizing the sulfonate obtained at the step (a) from an organic solvent; and (c) making the sulfonate obtained at the step (b) react with a base to conduct desalination, thereby conducting isolation as a free object.SELECTED DRAWING: None

Inventors:

HAN SHIN
JEON SEONG HYEON
LEE SHIN YOUNG

Application Number:

JP2017136251A

Publication Date:

February 15, 2018

Filing Date:

July 12, 2017

Export Citation:

Click for automatic bibliography generation Help

Assignee:

HEXAPHARMATEC CO LTD

International Classes:

C07D223/16

Attorney, Agent or Firm:

Ryu Iwatani

Previous Patent: [(2R, 3S, 4R, 5R) -5- (6- (cyclopentylamino) -9H-pudding 9- Il ) -3 and 4-dihydroxy tetrahydro franc...

Next Patent: A production method of 2, 3, 3, and 3-tetrafluoro pro pen