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HRID1050284

反应详情

EQUATION

反应方程式

HRID 1050284 的结构方程式

REACTANTS

反应物

2
结构：NN.O
HCID24654

Hydrazine hydrate (1:1)

H6N2O

结构：COc1ccc2c(c1)CC[C@@H]1[C@@H]2CC[C@]2(C)[C@H](O)[C@@H](N=[N+]=[N-])C[C@@H]12
HCID21723403

未命名化合物

PRODUCTS

生成物

1
结构：COc1ccc2c(c1)CC[C@@H]1[C@@H]2CC[C@]2(C)[C@H](O)[C@@H](N)C[C@@H]12
HCID15819151

(16β,17α)-16-Amino-3-methoxyestra-1,3,5(10)-trien-17-ol

C19H27NO2

AUXILIARIES

试剂、催化剂与溶剂

2
结构：[Ni]
催化剂HCID935

Nickel

Ni

结构：CO
溶剂HCID887

Methanol

CH4O

PROCEDURE

实验过程

1.0 g 16β-azido-3-methoxy-estra-1,3,5(10)-triene-17α-ol, 10 ml methanol, 2 ml 80% hydrazine hydrate and a spatula tip of Raney nickel are heated on a water bath for 15 min. After filtration, the Raney nickel is washed with methanol, subsequently wash fluid and filtrate are combined and methanol is removed by distillation under vacuum. The residue is recrystallized from methanol/ether. Yield: 0.8 g (87%), F=158-160° C.; [α]D+68° (pyridine).

WORKUP

后处理

  1. filtrationAfter filtration
  2. washthe Raney nickel is washed with methanol, subsequently wash fluid and filtrate
  3. custommethanol is removed by distillation under vacuum
  4. customThe residue is recrystallized from methanol/ether
  5. customYield: 0.8 g (87%), F=158-160° C.