HRID1510036

反应详情

EQUATION

反应方程式

HRID 1510036 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

8.9 g of 4-[4-(4-(benzyloxycarbonyl)piperazin-1-yl)phenyl]-3,4-dihydro-2H-quinoxaline-1-carboxylic acid tert-butyl ester are placed in 220 ml of dichloromethane. 55 ml of a 4N solution of hydrochloric acid in dioxane are slowly added at 0° C. The mixture is stirred for 5 minutes under cold conditions and then it is allowed to return to ambient temperature. The reaction mixture is stirred at ambient temperature for 18 h and is then diluted with dichloromethane. A saturated aqueous sodium carbonate solution is added and then the addition is continued with solid sodium carbonate until a pH=7-8 is reached. The aqueous phase is extracted with dichloromethane. The organic phases are combined, washed with water, dried over sodium sulphate, filtered through a sintered glass filter and concentrated under vacuum. 7.2 g of 4-[4-(3,4-dihydro-2H-quinoxalin-1-yl)phenyl]piperazine-1-carboxylic acid benzyl ester are obtained in the form of an oil.

WORKUP

后处理

  1. customto return to ambient temperature
  2. stirringThe reaction mixture is stirred at ambient temperature for 18 h
  3. additionthe addition
  4. extractionThe aqueous phase is extracted with dichloromethane
  5. washwashed with water
  6. dry with materialdried over sodium sulphate
  7. filtrationfiltered through a sintered glass
  8. filtrationfilter
  9. concentrationconcentrated under vacuum