反应详情

To a solution of 28.1 g (140 mmol) of 5 in 150 mL of dry diethyl ether, 25.6 g (8.89 mL, 94.4 mmol) of PBr3 was added at −10° C. The resulting mixture was stirred for 12 hr at room temperature and then added to 450 mL of cold water. The organic layer was separated, and the aqueous layer was extracted with 2×150 mL of water. The combined organic extracts were washed with aqueous NaHCO3, dried over Na2SO4, and then evaporated to dryness. This procedure gave 33.0 g (89%) of the title product.

1. customThe organic layer was separated
2. extractionthe aqueous layer was extracted with 2×150 mL of water
3. washThe combined organic extracts were washed with aqueous NaHCO3
4. dry with materialdried over Na2SO4
5. customevaporated to dryness