HRID1244167
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
To a solution of 4-(4-bromo-phenyl)-2-(2-ethoxycarbonyl-acetylamino)-thiophene-3-carboxylic acid ethyl ester (4.98 g, 11.3 mmol) in DMF (30 mL) at 0° C. was added a dispersion of sodium hydride in mineral oil (60%, 2.73 g, 68.2 mmol). After warming to ambient temperature the reaction was stirred overnight. Aqueous HCl (1.2 M, 100 mL) was added while cooling the mixture to 0° C. After stirring 1 h. the mixture was filtered and washed with H2O and hexanes giving the titled compound (2.85 g, 64%) as a gray solid.
WORKUP
后处理
- temperaturewhile cooling the mixture to 0° C
- stirringAfter stirring 1 h. the mixture
- filtrationwas filtered
- washwashed with H2O and hexanes giving the titled compound (2.85 g, 64%) as a gray solid