HRID216396

反应详情

EQUATION

反应方程式

HRID 216396 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Hydrogen chloride (4 M in dioxane) (1.5 mL, 0.67 mmol) was added to a solution of 2-[4-(2,2-dimethylbutyl)-1-trityl-1H-imidazol-2-yl]-1-[4-(5-fluoropyridin-2-yl)phenyl]ethanol (200 mg, 0.33 mmol) in methanol (6 mL). After stirring at ambient temperature for 3 h, volatiles were removed. The residue was partitioned between 1 N hydrochloric acid and diethyl ether. The aqueous phase was washed with diethyl ether, basified with saturated aqueous sodium carbonate and extracted with diethyl ether and ethyl acetate. Combined extracts were dried (magnesium sulfate) and concentrated in vacuo to afford the title compound. Purification by HPLC (Gilson; Chiralcel OJ column; 10 mL/min; 10% isopropanol/heptane). (M+H) found 368.

WORKUP

后处理

  1. customvolatiles were removed
  2. customThe residue was partitioned between 1 N hydrochloric acid and diethyl ether
  3. washThe aqueous phase was washed with diethyl ether
  4. extractionextracted with diethyl ether and ethyl acetate
  5. dry with materialCombined extracts were dried (magnesium sulfate)
  6. concentrationconcentrated in vacuo