反応 #2079

反応方程式

dehydroepiandrosterone

benzylchloroformate

→

3β-benzyloxycarbonyloxy-5-androsten-17-one

溶媒

methylene chloride

反応条件

後処理

1. 1
   洗浄the mixture is washed with water
2. 2
   その他evaporated to dryness
3. 3
   workup.DISSOLUTIONThe residue is then dissolved in acetone
4. 4
   その他precipitated in iced water
5. 5
   workup.WAITAfter 16 h
6. 6
   ろ過crystals are filtered
7. 7
   その他dried in vacuo

実験手順

To a stirred solution of dehydroepiandrosterone (2.88 % 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.

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