HRID974376

反应详情

EQUATION

反应方程式

HRID 974376 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of 1.0 g (6.2 mmoles) of 7-benzothiophene-carbaldehyde, 0.4 g (6.8 mmoles) of cyanoacetic acid methyl ester, 0.07 g of ammonium acetate, 0.2 g of acetic acid, 1 g of molecular sieve (3 Å) and 10 ml of toluene are boiled under reflux for 4 hours, and then the reaction mixture is cooled and mixed with 20 ml of ethyl acetate and with 20 ml of 10% NaCl solution. The separated organic phase is dried with MgSO4, filtered and the solvent is evaporated in vacuo. 1.5 g of 2-cyano-3-(benzothiophen-7-yl)-acrylic acid methyl ester in the form of a crude product is obtained as residue.

WORKUP

后处理

  1. temperatureunder reflux for 4 hours
  2. temperaturethe reaction mixture is cooled
  3. dry with materialThe separated organic phase is dried with MgSO4
  4. filtrationfiltered
  5. customthe solvent is evaporated in vacuo