反应详情

A solution of 19 (300 mg, 0.55 mmole) in dry THF (2 ml) was added to a suspension of LiAIH4 (105 mg, 2.75 mmole) in 5 ml of dry THF at 5° C. and stirred at room temperature for 1 hour. Na2SO4 /10H2O (2 g) was added to the reaction mixture and stirred for 15 hours at room temperature. The suspension was filtrated, and the solids were washed with dry THF. The filtrate was concentrated under reduced pressure. The resulting oil was dissolved in 2 ml of acetone, and CH3SO3H (159 mg, 1.65 mmole) was added to the solution of the crude oil in acetone (2 ml). The resulting precipitate was collected by filtration and dried in vacuo to give 20 (254 mg, 0.31 mmole, 57%).

1. stirringstirred for 15 hours at room temperature
2. filtrationThe suspension was filtrated
3. washthe solids were washed with dry THF
4. concentrationThe filtrate was concentrated under reduced pressure
5. dissolutionThe resulting oil was dissolved in 2 ml of acetone
6. filtrationThe resulting precipitate was collected by filtration
7. customdried in vacuo