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HRID848783

反应详情

EQUATION

反应方程式

HRID 848783 的结构方程式

REACTANTS

反应物

2
结构：[BH4-].[Na+]
HCID4311764

Sodium borohydride (Na(BH4))

H4BNa

结构：CO[C@H]1CC[C@H]2[C@@H]3CC[C@H]4CC(=O)CC[C@]4(C)[C@H]3CC[C@]12C
HCID11044935

未命名化合物

PRODUCTS

生成物

1
结构：CO[C@H]1CC[C@H]2[C@@H]3CC[C@H]4C[C@H](O)CC[C@]4(C)[C@H]3CC[C@]12C
HCID12836861

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CC(C)O
溶剂HCID3776

Isopropanol

C3H8O

PROCEDURE

实验过程

Sodium borohydride (0.37 gms.) is added to a mixture of 17β-methoxy-5α-androstan-3-one (3 gms.) and isopropylalcohol (95%, 35 ml.). The mixture is stirred at 20°-25° for one hour and then is concentrated to dryness. The residue is column chromatographed on a size C prepacked Merck silica gel column. Elution was performed with ethyl acetate:cyclohexane, 10:90. 6 Ml. fractions are collected. The appropriate fractions (TLC) are combined and concentrated to dryness. The residue is recrystallized from isopropyl ether to give 3α-hydroxy-17β-methoxy-5α-androstane, m.p. 164°-167°; IR (mull) 3290, 3220, 1120, 1110, 1005 cm-1 ; NMR (CDCl3) 0.72, 0.76, 0.9-2.0, 3.21, 3.3, and 4.01 δ and 3β-hydroxy-17β-methoxy-5α-androstane, m.p. 150°-152°; NMR (CDCl3) 0.75-2.0, 3.25, 3.37 and 3.6 δ.

WORKUP

后处理

  1. concentrationis concentrated to dryness
  2. customchromatographed on a size C
  3. washElution
  4. customfractions are collected
  5. concentrationconcentrated to dryness
  6. customThe residue is recrystallized from isopropyl ether