HRID1952646
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
- 220 °C
PROCEDURE
实验过程
A mixture of 3-Bromo-5-methyl-thiophene-2-carboxylic acid methyl ester (0.54 g, 2.3 mmol), and Copper cyanide (0.27 g, 2.99 mmol) in NMP (3 ml) was heated in a microwave at 220° C. for 30 min. The reaction mixture was cooled and diluted with EtOAc. The organic layer was washed with aqueous NH4OH, and brine, dried over sodium sulfate, filtered and evaporated. The solid residue was purified by column (0-20% EtOAc in hexane) to give 0.31 g (74%) white solid.
WORKUP
后处理
- temperatureThe reaction mixture was cooled
- washThe organic layer was washed with aqueous NH4OH, and brine
- dry with materialdried over sodium sulfate
- filtrationfiltered
- customevaporated
- customThe solid residue was purified by column (0-20% EtOAc in hexane)