反应 #1543060
ord-091485dbf80b4477bbf9b439170a0ffc
反应方程式
dehydroepiandrosterone
benzylchloroformate
→
3β-benzyloxycarbonyloxy-5-androsten-17-one
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1洗涤the mixture is washed with water
- 2其他evaporated to dryness
- 3workup.DISSOLUTIONThe residue is then dissolved in acetone
- 4其他precipitated in iced water
- 5workup.WAITAfter 16 h
- 6过滤crystals are filtered
- 7其他dried in vacuo
实验过程
To a stirred solution of dehydroepiandrosterone (2.88 g, 10 mmol) in methylene chloride (100 mL) is added dropwise benzylchloroformate, over a period of 30 min following the known procedure (F. Reber and T. Reichstein, Helv. Chim. Acta, 28, 1164, 1945). After stirring for 3 h, the mixture is washed with water and evaporated to dryness. The residue is then dissolved in acetone and precipitated in iced water. After 16 h, crystals are filtered and dried in vacuo.