HRID1532456
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
- 50 °C
PROCEDURE
实验过程
To 0.186 g (1.0 mmol) of 2-(phenylsulfonyl)ethanol, 3 ml of acetonitrile was added, followed by 0.19 g(1.1 mmol) of methanesulfonic anhydride and 0.56 ml (4.0 mmol) of triethylamine, and the mixture was stirred for 5 hours at an internal temperature of 50° C. Subsequently, 0.29 g (1.5 mmol) of 5-bromoindole, 0.011 g (0.05 mmol) of palladium acetate, and 0.067 g (0.22 mmol) of tri(o-tolyl)phosphine were added, and the mixture was then refluxed for 17 hours. After cooled to room temperature, the reaction mixture was concentrated and purified by column chromatography (hexane/ethyl acetate=70/30) to obtain 0.066 g of 5-[2-(phenylsulfonyl)ethenyl]indole. Yield: 23%.
WORKUP
后处理
- temperaturethe mixture was then refluxed for 17 hours
- temperatureAfter cooled to room temperature
- concentrationthe reaction mixture was concentrated
- custompurified by column chromatography (hexane/ethyl acetate=70/30)