反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 20 °C
PROCEDURE
实验过程
272 mg of N-[(1S,2R)-1-(3,5-difluorobenzyl)-2-hydroxy-3-({1-[3-(trifluoromethyl)phenyl]cyclopropyl}amino)propyl]-7-chloro-1-oxo-2-(1-propylbutyl)-1,2,3,4-tetrahydroisoquinoline-5-carboxamide are dissolved, under an argon atmosphere, in 5 cm3 of ethyl ether. 0.35 cm3 of a 4N solution of hydrochloric acid in dioxane is added, while stirring, at a temperature of 20° C. The reaction mixture is concentrated to dryness under reduced pressure (5 kPa). The residue is taken up with two lots of 10 cm3 of diisopropyl ether, concentrated to dryness under reduced pressure (5 kPa), and dried under vacuum at a temperature of 35° C. 277 mg of N-[(1S,2R)-1-(3,5-difluorobenzyl)-2-hydroxy-3-({1-[3-(trifluoromethyl)phenyl]cyclopropyl}amino)propyl]-7-chloro-1-oxo-2-(1-propylbutyl)-1,2,3,4-tetrahydroisoquinoline-5-carboxamide hydrochloride (1:1) are obtained in the form of a beige powder.
WORKUP
后处理
- concentrationThe reaction mixture is concentrated to dryness under reduced pressure (5 kPa)
- concentrationconcentrated to dryness under reduced pressure (5 kPa)
- customdried under vacuum at a temperature of 35° C