反应详情

136 g of 2-(2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole were dissolved in 125 ml of chloroform. 175 g of chlorosulphonic acid were added dropwise at 0° C., with stirring, and the reaction mixture was subsequently stirred at room temperature until the evolution of gas had ended. It was then poured into 750 g of ice-water, the phases were separated and the aqueous phase was extracted with chloroform. The combined organic phases were washed with ice-water and sodium hydrogencarbonate solution and dried over magnesium sulphate and the readily volatile components were removed on a rotary evaporator to give 133 g of product (=72% of theory). The melting point was 55° to 57° C. 19F NMR: -60.8 and -86.5 ppm. 1H NMR: 3.13 ppm.

1. stirringthe reaction mixture was subsequently stirred at room temperature until the evolution of gas
2. customthe phases were separated
3. extractionthe aqueous phase was extracted with chloroform
4. washThe combined organic phases were washed with ice-water and sodium hydrogencarbonate solution
5. dry with materialdried over magnesium sulphate
6. customthe readily volatile components were removed on a rotary evaporator