反応 #167759

反応方程式

compound 12

2-amino-4-[(1R)-1-({[(6S)-6-(5-chloro-2-methoxybenzyl)-3-(ethoxyimino)-7-oxo-1,4-diazepan-1-yl]carbonyl}amino)butyl]benzoic acid

p-toluenesulfonic acid monohydrate

→

title compound

2-amino-4-[(1R)-1-({[(6S)-6-(5-chloro-2-methoxybenzyl)-3-(ethoxyimino)-7-oxo-1,4-diazepan-1-yl]carbonyl}amino)butyl]benzoic acid sesquitosylate

溶媒

acetonitrile

acetonitrile

反応条件

後処理

1. 1
   温度the mixture was cooled to 0° C.
2. 2
   ろ過the precipitates were collected by filtration

実験手順

The compound 12 obtained at Step (2) (503 mg) was dissolved in acetonitrile (0.5 ml), p-toluenesulfonic acid monohydrate in an acetonitrile solution (0.69M, 2 ml) was added at 60° C., then the mixture was allowed to gradually cool to room temperature. After 3 hours, the mixture was cooled to 0° C. and further stirred for 1.5 hours, then the precipitates were collected by filtration to obtain the title compound (535 mg) as a colorless crystals.

出典