تفاعل #3010

معادلة التفاعل

triphenylsulfonium chloride

dichloromethane

4-trifluoromethylbenzenesulfonyl chloride

sodium carbonate

→

triphenylsulfonium 4 -trifluoromethylbenzenesulfonate

المذيبات

water

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwas heated
2. 2
   درجة الحرارةat reflux for 22 hours
3. 3
   workup.STIRRINGthe mixture stirred at room temperature for 20 hours
4. 4
   أخرىThe layers were separated
5. 5
   غسيلthe organic layer washed with water (7×150 ml) until the washings
6. 6
   أخرىAfter drying
7. 7
   أخرى(MgSO4 ), removal of the solvent in vacuo
8. 8
   أخرىgave a pale yellow foam which
9. 9
   أخرىwas further dried
10. 10
    درجة الحرارةby heating at 80°-100° C. for 108 hours under vacuum

الإجراء التجريبي

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).

المصدر