HRID14477

反应详情

EQUATION

反应方程式

HRID 14477 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A stirred solution of 7-amino-8-bromo-3-(4-chlorophenyl)-2-isopropyl-chromen-4-one (0.242 g, 0.62 mmol) in anhydrous methylene chloride (5 ml) is treated with a 20% solution of phosgene in toluene (0.5 ml). After 3 h, triethylamine (0.12 g, 0.17 ml, 1.24 mmol, 2 eq.) is added, followed by benzyl alcohol (0.067 g, 0.064 ml, 0.62 mmol), and the solution is stirred at room temperature overnight. The solution is diluted with methylene chloride and washed with water. The organic layer is dried (magnesium sulfate) and filtered, and the solvent is removed by evaporation in vacuo. The resulting solid is purified by flash chromatography (cyclohexane/ethyl acetate=9:1) to afford the title compound as a pale yellow solid.

WORKUP

后处理

  1. washwashed with water
  2. dry with materialThe organic layer is dried (magnesium sulfate)
  3. filtrationfiltered
  4. customthe solvent is removed by evaporation in vacuo
  5. customThe resulting solid is purified by flash chromatography (cyclohexane/ethyl acetate=9:1)