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HRID726169

反应详情

EQUATION

反应方程式

HRID 726169 的结构方程式

REACTANTS

反应物

4
结构：O
HCID962

Water

H2O

结构：[I-].[Na+]
HCID5238

Sodium Iodide

INa

结构：[N-]=[N+]=[N-].[Na+]
HCID33557

未命名化合物

结构：C[C@@H]1CC[C@@]2(OC1)O[C@H]1C=C3[C@@H]4CC[C@H]5CC(=O)C(Br)C[C@]5(C)[C@H]4CC(=O)[C@]3(C)[C@H]1[C@@H]2C
HCID15282201

未命名化合物

PRODUCTS

生成物

1
结构：C[C@@H]1CC[C@@]2(OC1)O[C@H]1C=C3[C@@H]4CC[C@H]5CC(=O)C(=N)C[C@]5(C)[C@H]4CC(=O)[C@]3(C)[C@H]1[C@@H]2C
HCID15282202

未命名化合物

收率 93.5%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CN(C)C=O
溶剂HCID6228

N,N-Dimethylformamide

C3H7NO

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

500 mg (0.99 mmol) of 2-bromo-(25R)-5α-spirost-14-ene-3,12-dione (II) is dissolved in 50 ml of dimethylformamide. After adding 700 mg of sodium azide and a few milligrams of sodium iodide, the solution is stirred for 2 hours at 50° C. The reaction mixture is brought to room temperature, poured into 20 ml of water and extracted with methyl-tert-butyl ether. This extract is washed with saturated sodium chloride solution, dried on magnesium sulfate and concentrated by evaporation. After crystallization, 407 mg (80%) of iminoketone III is obtained.

WORKUP

后处理

  1. customis brought to room temperature
  2. extractionextracted with methyl-tert-butyl ether
  3. washThis extract is washed with saturated sodium chloride solution
  4. customdried on magnesium sulfate
  5. concentrationconcentrated by evaporation
  6. customAfter crystallization