HRID1532458

反应详情

EQUATION

反应方程式

HRID 1532458 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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, 0.22 ml (1.5 mmol) of 1-iodonaphthalene, 0.11 g (0.05 mmol) of palladium acetate, and 0.067 g (0.22 mmol) of tri(o-tolyl)phosphine were added thereto, 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=80/20) to obtain 0.194 g of [2-(phenylsulfonyl)ethenyl]naphthalene. Yield: 66%.

WORKUP

后处理

  1. temperaturethe mixture was then refluxed for 17 hours
  2. temperatureAfter cooled to room temperature
  3. concentrationthe reaction mixture was concentrated
  4. custompurified by column chromatography (hexane/ethyl acetate=80/20)