HRID216369

反应详情

EQUATION

反应方程式

HRID 216369 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

Hydrogen chloride (4 M in 1,4-dioxane) (2 mL, 0.5 mmol) was added to an ambient temperature solution of 1-[4-(2,2-dimethylpropyl)-1-trityl-1H-imidazol-2-yl]-2-(4-isothiazol-5-ylphenyl)propan-2-ol (103 mg, 0.17 mmol) in methanol (4 mL). After stirring at 70° C. for 1 h, volatiles were removed in vacuo. The residue was basified with 10% aqueous sodium hydroxide and extracted with ethyl acetate. Combined extracts were dried (magnesium sulfate) and concentrated in vacuo. Chromatography over silica eluting with 0-100% acetone/methylene chloride afforded the title compound. LCMS: 356 (M+H). Individual enantiomer (E1 or E2) was obtained by HPLC separation on a chrial column.

WORKUP

后处理

  1. customvolatiles were removed in vacuo
  2. extractionextracted with ethyl acetate
  3. dry with materialCombined extracts were dried (magnesium sulfate)
  4. concentrationconcentrated in vacuo