HRID428950

反应详情

EQUATION

反应方程式

HRID 428950 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3-hexyl-6-methyl-6-[3-(1-triphenylmethyl-1H-imidazol-5-yl)phenyl]-3-azabicyclo[3.1.0]hexan-2-one (Preparation 74, 55 mg, 0.95 nmmol) in methanol (1.5 ml) was added aqueous hydrochloric acid (2M, 0.5 ml) and the mixture was heated under reflux for 16 h. The reaction mixture was then cooled to room temperature and poured onto solid sodium hydrogen carbonate. Dichloromethane was added, the layers were separated and the organic extracts were dried (MgSO4) and concentrated in in vacuo. The crude residue was chromatographed on silica gel eluting with ethyl acetate to give the title compound as a clear oil (21 mg, 66%).

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 16 h
  3. customthe layers were separated
  4. dry with materialthe organic extracts were dried (MgSO4)
  5. concentrationconcentrated in in vacuo
  6. customThe crude residue was chromatographed on silica gel eluting with ethyl acetate