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温度

0 °C

Under argon and in an anhydrous medium, 1.50 g (3.76 mmol) of 1.2-bis-diphenylphosphinoethane are added at 0° C. to a solution of 1.25 g (3.76 mmol) of carbon tetrabromide in 20 ml of dichloromethane. After 10 minutes at 0° C., 417 mg (1.88 mmol) of the compound obtained in Step D dissolved in 10 ml of dichloromethane are added to the mixture. The mixture is stirred for 30 minutes at 0° C., and then for 3 hours at room temperature. After hydrolysis of the reaction mixture, the organic phase is dried over magnesium sulphate, filtered and concentrated. Purification by flash chromatography over silica gel (eluant:petroleum ether/ethyl acetate, 8:2) yields the title compound in the form of a white solid.

1. additionare added to the mixture
2. waitfor 3 hours at room temperature
3. customAfter hydrolysis of the reaction mixture
4. dry with materialthe organic phase is dried over magnesium sulphate
5. filtrationfiltered
6. concentrationconcentrated
7. customPurification by flash chromatography over silica gel (eluant:petroleum ether/ethyl acetate, 8:2)