HRID725173

反应详情

EQUATION

反应方程式

HRID 725173 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 0.57 g of (1S,3aS,5S,7aR)-1-formyl-5-phenyl-7a-methylperhydroinden-3a-ol and 1.50 g of aminoguanidine hydrogencarbonate in 30 ml of 0.01N hydrochloric acid and 80 ml of dioxane was kept at room temperature for 3 days and then evaporated to dryness under reduced pressure. The crude product was purified by flash-chromatography (SiO2) using chloroform/methanol/28% ammonium hydroxide 78/20/2 as the eluant. The fractions containing the title compound were collected and evaporated to dryness. The residue was triturated with ethanol/ethyl acetate to give 0.48 g of the title compound (I-aa) as a white solid.

WORKUP

后处理

  1. customevaporated 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
  6. customThe residue was triturated with ethanol/ethyl acetate