反应详情

温度

5 °C

79 mg of N-[(1S,2R)-1-benzyl-2-hydroxy-3-({1-[3-(trifluoromethyl)phenyl]cyclopropyl}amino)propyl]-1-oxo-2-(1-propylbutyl)-1,2,3,4-tetrahydroisoquinoline-5-carboxamide are dissolved in 1.2 cm3 of ethyl ether at a temperature close to 20° C. 0.4 cm3 of a 2M hydrochloric acid solution in ethyl ether is added while stirring under argon, at a temperature of 5° C. The reaction mixture precipitates. The stirring is continued for 20 min, then is stopped in order to remove the supernatant. 5 cm3 of ethyl ether are again added. This operation is carried out twice. The last suspension is then concentrated under reduced pressure (5 kPa). 68 mg of N-[(1S,2R)-1-benzyl-2-hydroxy-3-({1-[3-(trifluoromethyl)phenyl]cyclopropyl}amino)propyl]-1-oxo-2-(1-propylbutyl)-1,2,3,4-tetrahydroisoquinoline-5-carboxamide hydrochloride (1:1) are obtained in the form of a white solid.

1. customclose to 20° C
2. customThe reaction mixture precipitates
3. customto remove the supernatant
4. addition5 cm3 of ethyl ether are again added
5. concentrationThe last suspension is then concentrated under reduced pressure (5 kPa)