반응 #3010

반응 방정식

triphenylsulfonium chloride

dichloromethane

4-trifluoromethylbenzenesulfonyl chloride

sodium carbonate

→

triphenylsulfonium 4 -trifluoromethylbenzenesulfonate

용매

water

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도at reflux for 22 hours
3. 3
   workup.STIRRINGthe mixture stirred at room temperature for 20 hours
4. 4
   기타The layers were separated
5. 5
   세척the organic layer washed with water (7×150 ml) until the washings
6. 6
   기타After drying
7. 7
   기타(MgSO4 ), removal of the solvent in vacuo
8. 8
   기타gave a pale yellow foam which
9. 9
   기타was further dried
10. 10
    온도by heating at 80°-100° C. for 108 hours under vacuum

실험 절차

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).

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