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HRID1077224

反应详情

EQUATION

反应方程式

HRID 1077224 的结构方程式

REACTANTS

反应物

3
结构：Cl
HCID313

Hydrochloric Acid

ClH

结构：O
HCID962

Water

H2O

结构：CC[C@]12CC[C@@H]3C4=C(CC(OC)=CC4)C(C)C[C@H]3[C@@H]1CC[C@@H]2O
HCID68144451

未命名化合物

PRODUCTS

生成物

1
结构：CC[C@]12CC[C@H]3[C@@H](C[C@H](C)C4=CC(=O)CC[C@@H]43)[C@@H]1CC[C@@H]2O
HCID68144548

未命名化合物

收率 31.4%

AUXILIARIES

试剂、催化剂与溶剂

2
结构：CO
溶剂HCID887

Methanol

CH4O

结构：O.[Cl-].[Na+]
溶剂HCID57417360

Sodium chloride; water

ClH2NaO

PROCEDURE

实验过程

Stir dl-3-methoxy-17β-hydroxy-6-methyl-13-ethylgona-2,5(10)-diene (1.0 g) in methanol (54 cc) containing concentrated hydrochloric acid (3.6 cc) and water (2.4 cc) under nitrogen for 1.5 hours. Pour into brine, extract with ether and isolate the crude product. Chromatograph on Grade I neutral alumina (50 g) and recrystallize from ether-hexane to obtain the title compound (0.30 g), m.p. 127°-130°, λ max. KBr 2.98 μ, 6.03 μ; λ max. EtOH 240 mμ (ε16,500).

WORKUP

后处理

  1. extractionextract with ether
  2. customisolate the crude product
  3. customChromatograph on Grade I neutral alumina (50 g) and recrystallize from ether-hexane