HRID41693

反应详情

EQUATION

反应方程式

HRID 41693 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5 g of 4-bromophenylpiperazine are placed in a 500 ml three-necked flask under a nitrogen atmosphere. 4.34 ml of triethylamine are added. The mixture is cooled in an ice bath and 3.24 ml of benzyl chloroformate are added. The mixture is allowed to return to ambient temperature. It is diluted with dichloromethane and then gentle hydrolysis is carried out. The aqueous phase is extracted with dichloromethane. The organic phases are combined, washed with a saturated NaCl solution, dried over sodium sulphate, then filtered through a sintered glass filter and concentrated under vacuum. 8.43 g of 4-(4-bromophenyl)piperazine-1-carboxylic acid benzyl ester are obtained.

WORKUP

后处理

  1. temperatureThe mixture is cooled in an ice bath
  2. customto return to ambient temperature
  3. customgentle hydrolysis
  4. extractionThe aqueous phase is extracted with dichloromethane
  5. washwashed with a saturated NaCl solution
  6. dry with materialdried over sodium sulphate
  7. filtrationfiltered through a sintered glass
  8. filtrationfilter
  9. concentrationconcentrated under vacuum