反应详情

温度

0 °C

1.50 g (9.61 mmol) of 2′,4′-difluoroacetophenone were dissolved at 0° C. in 8 ml of diethyl ether, and 38.4 ml (19.21 mmol) of a 0.5N solution of cyclopropylmagnesium bromide in tetrahydrofuran were slowly added dropwise. Stirring at 0° C. for 1 h was followed by warming to RT, and the reaction solution was mixed with water and ethyl acetate, and the phases were separated. The organic phase was washed with saturated aqueous sodium chloride solution and dried over sodium sulfate, and the solvents were removed in vacuo. The crude product was purified by preparative HPLC (mobile phase: acetonitrile-water gradient) to result in 0.63 g (33% of theory) of the title compound.

1. temperatureby warming to RT
2. customthe phases were separated
3. washThe organic phase was washed with saturated aqueous sodium chloride solution
4. dry with materialdried over sodium sulfate
5. customthe solvents were removed in vacuo
6. customThe crude product was purified by preparative HPLC (mobile phase: acetonitrile-water gradient)