HRID276818

反应详情

EQUATION

反应方程式

HRID 276818 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.1 g (4.8 mM) of 1-(2-aminoethyl)-4-(2-methoxyphenyl)-piperazine were added to 1.6 g (4.8 mM) of 2-ethoxymethyleneamino-3,5-dicarbethoxy-4,6-dihydrothieno[3,2-c]pyrrole in 25 ml of ethanol and refluxed for 2 h. The mixture was then concentrated in a rotary evaporator, and the crude product was purified by column chromatography (silica gel, mobile phase methylene chloride/methanol 96/4). After recrystallization from ethyl acetate, 1.1 g (47%) of product were isolated with melting point 153-155° C.

WORKUP

后处理

  1. temperaturerefluxed for 2 h
  2. concentrationThe mixture was then concentrated in a rotary evaporator
  3. customthe crude product was purified by column chromatography (silica gel, mobile phase methylene chloride/methanol 96/4)
  4. customAfter recrystallization from ethyl acetate