HRID435613

反应详情

EQUATION

反应方程式

HRID 435613 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

100 g of 2,10-dichloro-10,11dihydro-dibenzo[b,f]thiepin in 300 ml of chloroform are heated at reflux for 24 hours together with 182 g of 1-carbethoxy-piperazine. The mixture is then diluted with chloroform and water. The organic phase is washed several times with water and dried over magnesium sulphate. After filtration, the filtrate is concentrated under reduced pressure and the residue crystallised from acetone/hexane. There is obtained 1-carbethoxy-4-(2-chloro-10,11-dihydro-dibenzo[b,f]thiepin-10-yl)-piperazine of melting point 92°-93° C.

WORKUP

后处理

  1. washThe organic phase is washed several times with water
  2. dry with materialdried over magnesium sulphate
  3. filtrationAfter filtration
  4. concentrationthe filtrate is concentrated under reduced pressure
  5. customthe residue crystallised from acetone/hexane