HRID647441

反应详情

EQUATION

反应方程式

HRID 647441 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
160 °C

PROCEDURE

实验过程

A mixture of ethyl 2-{4-[N-(1,7-dichloroisoquinolin-3-yl)-N-methylamino]phenoxy}propionate (0.90 g), anhydrous potassium fluoride (1.50 g) and dry dimethyl sulfoxide (10 ml) was stirred at 160° C. for 48 hrs. The cooled mixture was dissolved in methylene chloride and washed repeatedly with water, then dried (MgSO4) and evaporated to give a crude, brown oil. Purification by column chromatography over silica gel (eluant: methylene chloride/hexane) gave Ethyl 2-{4-[N-(7-chloro-1-methylthioisoquinolin-3-yl)-N-methylamino]phenoxy}propionate (0.060 g) as a yellow oil and ethyl 2-{4-[N-(7-chloro-1-fluoroisoquinolin-3-yl)-N-methylamino]phenoxy}propionate (0.180 g) as a yellow oil.

WORKUP

后处理

  1. washwashed repeatedly with water
  2. dry with materialdried (MgSO4)
  3. customevaporated
  4. customto give a crude, brown oil
  5. customPurification by column chromatography over silica gel (eluant: methylene chloride/hexane)