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HRID725260

反应详情

EQUATION

反应方程式

HRID 725260 的结构方程式

REACTANTS

反应物

3
结构：Br
HCID260

Hydrogen Bromide

BrH

结构：Br.NNC1=NCCN1
HCID3085099

2-Hydrazino-delta-2-imidazoline hydrobromide

C3H9BrN4

结构：C/C(C=O)=C\[C@H]1CC[C@]2(O)[C@@H]3CC[C@@H]4C[C@@H](O)CC[C@]4(C)[C@H]3CC[C@]12C
HCID10666253

未命名化合物

PRODUCTS

生成物

1
结构：CC(/C=N/NC1=NCCN1)=C\[C@H]1CC[C@]2(O)[C@@H]3CC[C@@H]4C[C@@H](O)CC[C@]4(C)[C@H]3CC[C@]12C
HCID88140984

未命名化合物

收率 69.2%

AUXILIARIES

试剂、催化剂与溶剂

2
结构：O
溶剂HCID962

Water

H2O

结构：C1COCCO1
溶剂HCID31275

1,4-Dioxane

C4H8O2

2 次

PROCEDURE

实验过程

A solution of 0.55 g of 2-hydrazino-2-imidazoline hydrobromide in 10 ml of water and 30 ml of dioxane was made acid to pH 3 with 0.1N HBr. A solution of 1.00 g of (E)-3β,14β-dihydroxy-21-methyl-5β-pregn-20-ene-21-carboxaldehyde (Prepn, 1) in 10 ml of dioxane was added at room temperature. After 3 days, the solution was evaporated to dryness under reduced pressure. The crude product was purified by flash chromatography (SiO2) using chloroform/methanol/28% ammonium hydroxide 90/10/1 as the eluant: the fractions containing the title compound were collected and evaporated to dryness. The residue was ground with ethyl acetate and ethanol to give 0.85 g of the title compound (I-ab) as a white solid.

WORKUP

后处理

  1. customthe solution was evaporated to dryness under reduced pressure
  2. customThe crude product was purified by flash chromatography (SiO2)
  3. additionthe fractions containing the title compound
  4. customwere collected
  5. customevaporated to dryness