反应详情

温度

-70 °C

2-Bromoacetyl-1,4-benzodioxan(53.8 g) in methanol (500 mls) was cooled to -70° C. Sodium borohydride (10.3 g) was added and the solution stirred at -70° C. for 12 hours. The solution was treated with hydrobromic acid until acidic and the solvent evaporated. The residue was dissolved in ether and the ether extracts were washed with sodium bicarbonate solution; then water and dried (MgSO4) and evaporated to give a white solid. This was recrystallised eight times from petroleum spirit 60-80 to give 14 grams of the title compound.

1. customevaporated
2. dissolutionThe residue was dissolved in ether
3. washthe ether extracts were washed with sodium bicarbonate solution
4. dry with materialthen water and dried (MgSO4)
5. customevaporated
6. customto give a white solid
7. customThis was recrystallised eight times from petroleum spirit 60-80