HRID1668730

反应详情

EQUATION

反应方程式

HRID 1668730 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of 4-[1-(3-bromo-phenyl)-vinyl]-phenol (1.5 g, 5.45 mmol, 1.0 eq) in dichloromethane (15 mL), triethylamine (2.26 mL, 16.35 mmol, 3.0 eq) was added and the reaction mixture cooled to 0° C. Then methanesulfonyl chloride (0.465 mL, 6.0 mmol, 1.1 eq) was added dropwise and the mixture was allowed to warm to room temperature and stirred 16 h. The reaction was examined by TLC (ethyl acetate/cyclohexane 20%) which showed complete conversion to the desired product. After night time water was added and organic and water phase were separated. Organic solution was dried over magnesium sulfate filtered and evaporated. The crude was purified by flash chromatography eluting with cyclohexane, then ethyl acetate/cyclohexane 20%. 1.6 g of clean product was obtained as colorless liquid (yield: 65%).

WORKUP

后处理

  1. temperatureto warm to room temperature