HRID1248993

反应详情

EQUATION

反应方程式

HRID 1248993 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1-(2,4-dichlorophenyl)-2-(4-methylphenyl)propen-1-one (660 mg) and imidazole (770 mg) in ethanol (10 ml) were stirred at room temperature for 16 hours. The reaction mixture was concentrated under reduced pressure, dissolved in ethyl acetate, washed with water, dried over anhydrous magnesium sulphate and concentrated under reduced pressure to yield a gum. The gum was chromatographed on silica gel in methanol: dichloromethane (1:24) to yield 1-(2,4-dichlorophenyl)-3-(imidazol-1-yl)-2-(4-methylphenyl)propan-1-one (450 mg) (Found: C, 78.25; H, 5.88; N, 9.53; C19H18N2O requires C, 78.62; H, 6.21; N, 9.66) which was treated with ethereal hydrogen chloride to yield the hydrochloride salt of 1-(2,4-dichlorophenyl)-3-(imidazol-1-yl)-2-(4-methylphenyl)propan-1-one m.p. 92°-96° C. (Found: C, 54.79; H, 4.33; N, 6.59; C19H17Cl3N2O.H2O requires C, 55.16; H, 4.38; N, 6.77) having the formula: ##STR25##

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. dissolutiondissolved in ethyl acetate
  3. washwashed with water
  4. dry with materialdried over anhydrous magnesium sulphate
  5. concentrationconcentrated under reduced pressure
  6. customto yield a gum
  7. customThe gum was chromatographed on silica gel in methanol: dichloromethane (1:24)