反应详情

A solution of (3) (2.4 g, 8.6 mmol) in tetrahydrofuran (40 ml) was added 60% NaH (0.69 g, 17 mmol) and stirred at room temperature for one hour. Diethyl sulfate (1.4 ml, 11 mmol) was added and the reaction mixture stirred over night. Water was added and the reaction mixture was extracted with diethyl ether (3×40 ml). The combined organic phases was dried with magnesium sulfate and evaporated to dryness. Column chromatography, using a mixture of dichloromethane, methanol and ammonia (aq) (9:1:1%) yielded 1.5 g (56%) of product (9) (oil).

1. stirringthe reaction mixture stirred over night
2. extractionthe reaction mixture was extracted with diethyl ether (3×40 ml)
3. dry with materialThe combined organic phases was dried with magnesium sulfate
4. customevaporated to dryness
5. additiona mixture of dichloromethane, methanol and ammonia (aq) (9:1:1%)