反应详情

Hydroxylamine hydrochloride (3.48 g) and triethylamine (7 ml) were stirred for 0.25 hours in DMF (50 ml) at 0° C. tert-Butyldiphenylsilyl chloride (13 ml) was added and the mixture was stirred for 1 hour. The mixture was partitioned between pentane (500 ml) and water (100 ml), the layers separated and the aqueous phase extracted with ethyl acetate (2×100 ml). The organic layers were combined, washed with brine (50 ml), dried over magnesium sulphate and the solvent was removed in vacuo. The crude product was triturated with pentane (20 ml) yielding the pure title compound as white solid (4.04 g), m.p.t. 85°-87° C.

1. additionwas added
2. customThe mixture was partitioned between pentane (500 ml) and water (100 ml)
3. customthe layers separated
4. extractionthe aqueous phase extracted with ethyl acetate (2×100 ml)
5. washwashed with brine (50 ml)
6. dry with materialdried over magnesium sulphate
7. customthe solvent was removed in vacuo
8. customThe crude product was triturated with pentane (20 ml)