反应详情

A solution of 1.19 g of 2-hydrazino-2-imidazoline hydrobromide in 20 ml of water and 60 ml of dioxane was made acid to pH 3 with 0.1N HBr. A solution of 2.08 g of (E)-3β,14β-dihydroxy-5β-pregn-20-ene-21-carboxaldehyde (Fullerton D. S. et al., J. Med. Chem., 1976, 19, 1330) in 25 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 1.54 g of the title compound (I-ac) as a white solid.

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