HRID1359984

反应详情

EQUATION

反应方程式

HRID 1359984 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The Boc-aminopropanol-fenbufen obtained above (1.82 mmol) was dissolved in dichloromethane (4 ml), and under ice-cooling, 4 N hydrochloric acid ethyl acetate solution (4 ml) was added thereto, and then the mixture was gradually returned to room temperature and stirred for 90 minutes. Precipitation of white precipitate was observed just after the commencement of the reaction. After confirming disappearance of Boc-aminopropanol-fenbufen by TLC, diethyl ether was added to the reaction solution, and the resulting white precipitate was centrifuged. The precipitate was washed three times with diethyl ether and then dried under reduced pressure to give the titled compound (621.4 mg, yield 98%). The structure was identified by 1H-NMR (CDCl3:CD3OD=1:1).

WORKUP

后处理

  1. temperatureunder ice-cooling
  2. customwas gradually returned to room temperature
  3. customPrecipitation of white precipitate
  4. customafter the commencement of the reaction
  5. additionwas added to the reaction solution
  6. washThe precipitate was washed three times with diethyl ether
  7. customdried under reduced pressure