反応 #3010

反応方程式

triphenylsulfonium chloride

dichloromethane

4-trifluoromethylbenzenesulfonyl chloride

sodium carbonate

→

triphenylsulfonium 4 -trifluoromethylbenzenesulfonate

溶媒

water

反応条件

後処理

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
   その他The layers were separated
5. 5
   洗浄the organic layer washed with water (7×150 ml) until the washings
6. 6
   その他After drying
7. 7
   その他(MgSO4 ), removal of the solvent in vacuo
8. 8
   その他gave a pale yellow foam which
9. 9
   その他was further dried
10. 10
    温度by heating at 80°-100° C. for 108 hours under vacuum

実験手順

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).

出典