反应详情

温度

0 °C

To a solution of compound 32 (84 g, 0.528 mol) in dry DMF (500 mL) was added triphenylphosphine (207 g, 0.79 mol) with vigorous stirring until it becomes a clear solution. The mixture was cooled to 0° C. and added CBr4 (260 g, 0.79 mol) portion wise over a period of 30 min and allowed to stir at RT for 5 h. The reaction mixture was cooled to 0° C., added saturated NaHCO3 solution (200 mL) and extracted with hexane (4×200 mL). The combined organic layer was dried, concentrated under vacuum and the crude title compound (117 g) was used for next reaction without any purification. TLC: Pet. ether/EtOAc, 7:3, Rf=0.6

1. stirringto stir at RT for 5 h
2. temperatureThe reaction mixture was cooled to 0° C.
3. extractionextracted with hexane (4×200 mL)
4. customThe combined organic layer was dried
5. concentrationconcentrated under vacuum
6. customthe crude title compound (117 g) was used for next reaction without any purification