HRID974376
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
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
- temperatureunder reflux for 4 hours
- temperaturethe reaction mixture is cooled
- dry with materialThe separated organic phase is dried with MgSO4
- filtrationfiltered
- customthe solvent is evaporated in vacuo