HRID216369
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customvolatiles were removed in vacuo
- extractionextracted with ethyl acetate
- dry with materialCombined extracts were dried (magnesium sulfate)
- concentrationconcentrated in vacuo