反应 #1543061

反应方程式

dehydroepiandrosterone

sodium acetate

Methylene chloride

L-cysteine ethyl ester hydrochloride

L-cysteine ethyl ester hydrochloride

→

3β-hydroxy-5-androstene

溶剂

ethanol

反应条件

后处理

1. 1
   温度the mixture is heated overnight under an argon atmosphere
2. 2
   过滤The solution is then filtered
3. 3
   洗涤the filtrate is washed twice with water
4. 4
   其他dried on magnesium sulfate
5. 5
   过滤filtered
6. 6
   其他evaporated under vacuum
7. 7
   其他The residue is triturated with ethanol
8. 8
   其他to give crystals

实验过程

Following the procedure described by Djerassi (C. Djerassi, N. Crossley and M. A. Kielczewski, J. Org. Chem. 27, 1112, 1962), dehydroepiandrosterone (2.88 g, 10 mmol) is dissolved in anhydrous ethanol, sodium acetate is added followed by L-cysteine ethyl ester hydrochloride (18 g, 100 mmol) and the mixture is heated overnight under an argon atmosphere. The reaction mixture is then evaported under vacuum. Methylene chloride is added to precipitate excess of L-cysteine ethyl ester hydrochloride. The solution is then filtered and the filtrate is washed twice with water, dried on magnesium sulfate, filtered and evaporated under vacuum. The residue is triturated with ethanol to give crystals.

来源