反应 #3010

反应方程式

triphenylsulfonium chloride

dichloromethane

4-trifluoromethylbenzenesulfonyl chloride

sodium carbonate

→

triphenylsulfonium 4 -trifluoromethylbenzenesulfonate

溶剂

water

反应条件

后处理

1. 1
   温度was heated
2. 2
   温度at reflux for 22 hours
3. 3
   workup.STIRRINGthe mixture stirred at room temperature for 20 hours
4. 4
   其他The layers were separated
5. 5
   洗涤the organic layer washed with water (7×150 ml) until the washings
6. 6
   其他After drying
7. 7
   其他(MgSO4 ), removal of the solvent in vacuo
8. 8
   其他gave a pale yellow foam which
9. 9
   其他was further dried
10. 10
    温度by heating at 80°-100° C. for 108 hours under vacuum

实验过程

A suspension of 4-trifluoromethylbenzenesulfonyl chloride (20.53 g, 83.9 mmol) in water (150 ml) containing sodium carbonate (9.43 g, 88.10 mmol) was heated at reflux for 22 hours. After cooling to room temperature, triphenylsulfonium chloride (50% aqueous solution, 50.00 g) was added over 15 minutes. After stirring the biphasic mixture for 30 minutes, dichloromethane (300 ml) was added and the mixture stirred at room temperature for 20 hours. The layers were separated and the organic layer washed with water (7×150 ml) until the washings were neutral (pH 7 ). After drying (MgSO4 ), removal of the solvent in vacuo gave a pale yellow foam which was further dried by heating at 80°-100° C. for 108 hours under vacuum. In this way, triphenylsulfonium 4 -trifluoromethylbenzenesulfonate was isolated as a pale yellow glass (36.77 g).

来源