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HRID1390765

反应详情

EQUATION

反应方程式

HRID 1390765 的结构方程式

REACTANTS

反应物

3
结构：O=C([O-])C(O)C(O)C(=O)[O-].[K+].[Na+]
HCID9855836

Potassium sodium tartarate

C4H4KNaO6

结构：CC(C)(C)[O][Al]([O]C(C)(C)C)[O]C(C)(C)C.[H-].[Li+]
HCID16710494

Lithium tri-tert-butoxyaluminohydride

C12H28AlLiO3

结构：CC(=O)O.CC(=O)O.C[C@@H]1C=C2CC(=O)C[C@H](C)[C@]2(CO)[C@H]2CC[C@]3(C)[C@@H](O)CC[C@H]3[C@H]12
HCID86736313

未命名化合物

PRODUCTS

生成物

1
结构：CC(=O)OC[C@]12C(=C[C@@H](C)[C@H]3[C@@H]4CC[C@H](OC(C)=O)[C@@]4(C)CC[C@@H]31)C[C@@H](O)C[C@@H]2C
HCID70604847

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：C1CCOC1
溶剂HCID8028

Tetrahydrofuran

C4H8O

2 次

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

To a solution of lithium tri-t-butoxyaluminum hydride in tetrahydrofuran is added a tetrahydrofuran solution of 17β,19-dihydroxy-1α,7α-dimethyl-5-androsten-3-one diacetate. The resulting mixture is stirred at 20° C. for a period of 18 hours after which is added an aqueous solution of sodium potassium tartrate. The mixture is filtered and concentrated to a small volume under reduced pressure. The concentrate is taken up in ether and washed well with water. The combined ether extracts are dried over magnesium sulfate, filtered and the ether removed under vacuum to yield a residue which when crystallized from a mixture of acetone-hexane results in the preparation of the desired 1α,7α-dimethyl-androst-5-ene-3β,17β,19-triol 17,19-diacetate.

WORKUP

后处理

  1. filtrationThe mixture is filtered
  2. concentrationconcentrated to a small volume under reduced pressure
  3. washwashed well with water
  4. dry with materialThe combined ether extracts are dried over magnesium sulfate
  5. filtrationfiltered
  6. customthe ether removed under vacuum
  7. customto yield a residue which when
  8. customcrystallized from a mixture of acetone-hexane