反应详情

123 ml (0.68 mol) Tris(dimethylamino)phosphine in 100 ml diglyme was added slowly dropwise to a solution of 26.3 ml (0.34 mol) dibromodifluoromethane in 800 ml diglyme. After stirring for one hour on an ice bath, 43 g (0.17 mol}benzyl 7-oxooctanoate in 100 ml diglyme was slowly added dropwise. The ice bath was removed and the reaction mixture stirred for 40 minutes at room temperature, poured into 1 liter ice-water and extracted with ether. The ether phase was washed twice with water, dried over sodium sulphate, filtered and concentrated. The residue was purified by column chromatography (silica gel hexane/ether=3:1)

1. customThe ice bath was removed
2. stirringthe reaction mixture stirred for 40 minutes at room temperature
3. additionpoured into 1 liter ice-water
4. extractionextracted with ether
5. washThe ether phase was washed twice with water
6. dry with materialdried over sodium sulphate
7. filtrationfiltered
8. concentrationconcentrated
9. customThe residue was purified by column chromatography (silica gel hexane/ether=3:1)