HRID1650799

反应详情

EQUATION

反应方程式

HRID 1650799 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-difluorophenyl)-2-(3-formyl-1,2,4-triazol-1-yl)-1-(1,2,4-triazol-1-ylmethyl)ethanol (0.6 g), p-methoxybenzyl-triphenylphosphonium chloride (1.68 g), potassium carbonate (0.5 g) and methanol (10 ml) was heated at 60°-70° for 2 hours, then left at room temperature for 20 hours. The reaction mixture was filtered, the separated solids were washed with methanol, and the combined organic solutions were evaporated to dryness. The residue was purified by medium pressure liquid chromatography on silica, eluting with chloroform, to give 1-(2,4-difluorophenyl)-2-[3-(4-methoxystyryl)-1,2,4-triazol-1-yl]-1-(1,2,4-triazol-1-ylmethyl)ethanol, m.p. 150°-152°.

WORKUP

后处理

  1. temperaturewas heated at 60°-70° for 2 hours
  2. filtrationThe reaction mixture was filtered
  3. washthe separated solids were washed with methanol
  4. customthe combined organic solutions were evaporated to dryness
  5. customThe residue was purified by medium pressure liquid chromatography on silica
  6. washeluting with chloroform