HRID1952595
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
- 115 °C
PROCEDURE
实验过程
A mixture of 5-Bromomethyl-3-chloro-thiophene-2-carboxylic acid methyl ester (3.8 g, 14.1 mmol) and NaHCO3 (20 g, 238 mmol) in DMSO (100 ml) was heated at 115° C. for 4 h. The reaction mixture was cooled. The reaction mixture was diluted with water and extracted with DCM (3×100 mL), washed with brine, dried over sodium sulfate, filtered and evaporated. The residue was purified by column (0-30% EtOAc in hexane) to give 1.30 g (45%) product.
WORKUP
后处理
- temperatureThe reaction mixture was cooled
- extractionextracted with DCM (3×100 mL)
- washwashed with brine
- dry with materialdried over sodium sulfate
- filtrationfiltered
- customevaporated
- customThe residue was purified by column (0-30% EtOAc in hexane)