HRID647441
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- washwashed repeatedly with water
- dry with materialdried (MgSO4)
- customevaporated
- customto give a crude, brown oil
- customPurification by column chromatography over silica gel (eluant: methylene chloride/hexane)