反応 #1062401

反応方程式

2,2,2-trifluoro-1-(4-trifluoromethylphenyl)ethanol

sodium hypochlorite

water

→

4-Trifluoroacetyltrifluoromethylbenzene

溶媒

methylene chloride

反応条件

後処理

1. 1
   その他are metered in within 20 minutes
2. 2
   workup.STIRRINGthe mixture is stirred for a further 5 hours at room temperature
3. 3
   その他the phases are separated
4. 4
   抽出the aqueous phase is extracted several times with methylene chloride
5. 5
   洗浄the combined organic phases are washed with saturated aqueous sodium chloride solution
6. 6
   乾燥After drying the organic phase with sodium sulfate
7. 7
   workup.DISTILLATIONthe volatiles are distilled off
8. 8
   workup.DISTILLATIONdistillation of the crude product (18 torr, 60°-61° C.), 16.74 g (66.5% of theory) of 4-trifluoroacetyltrifluoromethylbenzene
9. 9
   その他are obtained

実験手順

25.4 g (0.1 mol) of 2,2,2-trifluoro-1-(4-trifluoromethylphenyl)ethanol and 1.76 g (0.005 mol) of tetrabutylammonium hydrogen sulfate are dissolved in 350 ml of methylene chloride at room temperature. 108 ml (0.125 mol) of an approximately 12% strength sodium hypochlorite solution are metered in within 20 minutes with vigorous stirring and the mixture is stirred for a further 5 hours at room temperature. The reaction mixture is added to 400 ml of water, the phases are separated, the aqueous phase is extracted several times with methylene chloride and the combined organic phases are washed with saturated aqueous sodium chloride solution. After drying the organic phase with sodium sulfate, the volatiles are distilled off. Following distillation of the crude product (18 torr, 60°-61° C.), 16.74 g (66.5% of theory) of 4-trifluoroacetyltrifluoromethylbenzene are obtained, which, according to GC, is 96.7% pure. nD20 : 1.4146.

出典