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HRID1655647

反应详情

EQUATION

反应方程式

HRID 1655647 的结构方程式

REACTANTS

反应物

2
结构：CC(=O)OC(C)=O
HCID7918

Acetic anhydride

C4H6O3

结构：C[C@]12[C@@H](CC[C@H]3[C@@H]4[C@@H](O)CC(=O)[C@@]4(C)CC[C@@H]31)CC(=O)C[C@@]2(C)O
HCID67860436

未命名化合物

PRODUCTS

生成物

1
结构：CC(=O)O[C@H]1CC(=O)[C@@]2(C)CC[C@H]3[C@@H](CC[C@H]4CC(=O)C[C@@](C)(O)[C@@]43C)[C@H]12
HCID67860661

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

2
结构：c1ccncc1
溶剂HCID1049

Pyridine

C5H5N

结构：CCOC(C)=O
溶剂HCID8857

Ethyl acetate

C4H8O2

PROCEDURE

实验过程

20 ml of acetic anhydride is instilled at room temperature in 10.0 g of 1β,15α-dihydroxy-1α-methyl-5α-androstane-3,17-dione in 40 ml of pyridine. The reaction mixture is stirred into ice/water after 2.5 hours. The precipitated product is suctioned off, dissolved in ethyl acetate and washed neutral with water. The crude product is chromatographed on silica gel with a hexane-ethyl acetate gradient. 8.6 g of 15α-acetoxy-1β-hydroxy-1α-methyl-5α-androstane-3,17-dione is obtained. Melting point 170.0° C.

WORKUP

后处理

  1. washwashed neutral with water
  2. customThe crude product is chromatographed on silica gel with a hexane-ethyl acetate gradient