HRID441986

反应详情

EQUATION

反应方程式

HRID 441986 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

17.6 g of 10-chloro-8-fluoro-10,11-dihydro-2-methyl-dibenzo[b,f]thiepin are heated for 20 hours under reflux conditions together with 27.3 g of 3-[2-(1-piperazinyl)-ethyl]-2-oxazolidinone in 100 ml of chloroform. After evaporation of the chloroform, the residue is mixed with ice, benzene and aqueous sodium hydroxide solution and again mixed well. The benzene phase is acidified with 6 N aqueous hydrochloric acid and maintained in an ice bath for 30 minutes. The precripitate, which is formed, is filtered, made alkaline with aqueous sodium hydroxide solution and taken up in benzene. The benzene phase is dried over sodium sulphate and evaporated, whereby 3-{2-[4-(8-fluoro-10,11-dihydro-2-methyl-dibenzo [b,f]thiepin-10-yl)-1-piperazinyl]-ethyl}-2-oxazolidinone is obtained, which is converted into the corresponding dihydrochloride by reaction with ethanolic hydrochloric acid. The dihydrochloric melts at 210° (dec;).

WORKUP

后处理

  1. customAfter evaporation of the chloroform
  2. additionthe residue is mixed with ice, benzene and aqueous sodium hydroxide solution
  3. additionagain mixed well
  4. temperaturemaintained in an ice bath for 30 minutes
  5. customThe precripitate, which is formed
  6. filtrationis filtered
  7. dry with materialThe benzene phase is dried over sodium sulphate
  8. customevaporated