HRID129633
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
- -15 °C
PROCEDURE
实验过程
Trifluoromethanesulfonic acid (0.27 g, 0.001795 mol) is added to a solution of methyl 5-(p-chlorophenyl)pyrrole-2-carboxylate (4.23 g, 0.01795 mol) in methylene chloride (70 mL) at -30° C. This mixture is treated with trifluoromethylsulfenyl chloride (4.0 g, 0.0293 mol), stirred for 30 minutes at -15° C., warmed to room temperature with stirring for three hours, diluted with methylene chloride, washed with saturated sodium hydrogen carbonate solution and brine, dried over anhydrous magnesium sulfate and concentrated in vacuo to obtain the title product as an off-white solid (5.44 g, mp 133°-137° C.) which is identified by 1HNMR spectral analysis.
WORKUP
后处理
- temperaturewarmed to room temperature
- stirringwith stirring for three hours
- washwashed with saturated sodium hydrogen carbonate solution and brine
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated in vacuo