反应详情

温度

25 °C

4-Fluoro-2-(trifluoromethyl)benzenesulphonyl chloride (2.0 g) was dissolved in dioxane (12 mL) under a N2-atmosphere at ambient temperature. Water (3.0 mL) and tris-(2-carboxylethyl)phosphine hydrochloride (8.73 g) was added afterwards. The reaction mixture is stirred under reflux for 6 h. The reaction mixture is cooled to 25° C. and dissolved with water (30 mL). The product is extracted with CH2Cl2 (100 mL) several times. The combined organic layers are washed with water and dried over Na2SO4. The organic layer is filtrated and evaporated to dryness to yield 1.27 g (85%) of a colorless liquid which is used without further purification. MS (ESI): m/z=194.9 [M−H]−.

1. temperatureunder reflux for 6 h
2. extractionThe product is extracted with CH2Cl2 (100 mL) several times
3. washThe combined organic layers are washed with water
4. dry with materialdried over Na2SO4
5. filtrationThe organic layer is filtrated
6. customevaporated to dryness