反应详情

A solution of ethyl methanesulfonate (4.27 mL, 40.3 mmol) in 100 mL of dry THF was treated at -78° C. with 19.3 mL (44.4 mmol) of n-BuLi in hexane. After 15 min. diethyl chlorophosphate (3.30 ml, 22.2 mmol) was added. The solution was kept at -78° C. for 0.5 h and allowed to stay at -50° C. for 1 h. Saturated ammonium chloride (75 mL) was added to the solution and the mixture warmed to room temperature. The mixture was concentrated (THF removed), diluted with water and extracted with methylene chloride (3×70 mL). The combined organic fractions were dried (MgSO4), concentrated and purified by distillation to yield 3.86 g (70%) of title compound.

1. waitto stay at -50° C. for 1 h
2. concentrationThe mixture was concentrated
3. custom(THF removed)
4. additiondiluted with water
5. extractionextracted with methylene chloride (3×70 mL)
6. dry with materialThe combined organic fractions were dried (MgSO4)
7. concentrationconcentrated
8. distillationpurified by distillation