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., while stirring, and the mixture was subsequently stirred at room temperature until the evolution of gas had ended. It was then poured onto 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 bicarbonate solution, dried with magnesium sulphate and freed from readily volatile constituents on a rotary evaporator. 133 g of product were obtained (=72% of theory), and the melting point was 55° to 57° C. 19F-NMR: -60.8 and -86.5 ppm. 1H-NMR: 3.13 ppm.

1. stirringthe 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 bicarbonate solution
5. dry with materialdried with magnesium sulphate
6. customfreed from readily volatile constituents on a rotary evaporator