反应详情

温度

65 °C

To a solution of the azide of Example 51 (11-3) (6.46 g, 40.6 mmol) in methanol (100 ml) was added hydroxylamine hydrochloride (3.95 g, 56.84 mmol), followed by triethylamine (9.6 ml). The solution was heated to 65° C. for four hours. The solvent was removed under reduced pressure and the remaining residue was extracted with ethylacetate (300 ml) and water (100 ml). The water layer was re-extracted with ethylacetate (2×200 ml). The combined organic extracts were washed with brine (2×100 ml), dried over MgSO4 and evaporated to yield the title product (11-4) (7.8 g).

1. customThe solvent was removed under reduced pressure
2. extractionthe remaining residue was extracted with ethylacetate (300 ml) and water (100 ml)
3. extractionThe water layer was re-extracted with ethylacetate (2×200 ml)
4. washThe combined organic extracts were washed with brine (2×100 ml)
5. dry with materialdried over MgSO4
6. customevaporated