HRID1073949

反应详情

EQUATION

反应方程式

HRID 1073949 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

580 mg of 4-[1,1-dimethyl-3-(2-pyrimidinyl)-2-pro pynyloxy]benzonitrile were heated at reflux for 3 hours in 20 ml of dichlorobenzene. The solution was allowed to cool and was then evaporated to dryness. The residue was chromatographed on silica gel using ethyl acetate/petroleum ether (1:2) and subsequently ethyl acetate/petroleum ether (1:1) for the elution. There was obtained 361 mg of 2,2-dimethyl-4-(2-pyrimidinyl)-2H-1-benzopyran-6-carbonitrile which melted at 108°-109.5° C. after recrystallization from tert-butyl methyl ether.

WORKUP

后处理

  1. temperatureto cool
  2. customwas then evaporated to dryness
  3. customThe residue was chromatographed on silica gel
  4. washfor the elution