137977-97-0Relevant articles and documents
Preparation method for tolvaptan intermediate
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Paragraph 0019-0021; 0022, (2018/09/08)
The invention discloses a preparation method for a tolvaptan intermediate. The tolvaptan intermediate is obtained by performing catalytic hydrogenation on 1-(4-nitro-2-methylbenzoyl)-7-chloro-5-oxo-2,3,4,5-tetrahydro-1H-1-benzazepine in an organic solvent to obtain 1-(4-amino-2-methylbenzoyl)-7-chloro-5-oxo-2,3,4,5-tetrahydro-1H-1-benzazepine; a catalytic system adopted by the catalytic hydrogenation is a metal chloride + a palladium carbon catalyst; and the metal chloride is lithium chloride or indium trichloride. The method provided by the invention adopts LiCl/InCl3 + the palladium carbon catalyst as the catalytic hydrogenation system, and the catalytic hydrogenation system can not only obtain a higher reaction yield, but also can effectively avoid an occurrence of a dechlorination reaction, thereby obtaining higher product purity; and the method provided by the invention has less pollution to the environment and lower production costs, and is suitable for industrialized production.
METHOD FOR PURIFYING 1-(4-AMINO-2-METHYLBENZOYL)-7-CHLORO-5-OXO-2,3,4,5-TETRAHYDRO-1H-1-BENZAZEPINE
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Paragraph 0020, (2018/04/06)
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 COPYRIGHT: (C)2018,JPOandINPIT
A the request cuts down the Pu Tanzania intermediate and its preparation method
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Paragraph 0033; 0034; 0035; 0036; 0037; 0038; 0039-0044, (2017/06/28)
The invention relates to the field of pharmaceutical chemistry and particularly discloses preparation methods for a tolvaptan intermediate 1-(4-amino-2-methylbenzoyl)-7-chloro-5-oxo-2,3,4,5-tetrahydro-1H-1-benzoazepine (I) (shown in the description) and salts thereof. The tolvaptan intermediate prepared by utilizing the method disclosed by the invention has the characteristics of low cost, high yield, environmental friendliness, strong operability and suitability for industrial production.