HRID1650799
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas heated at 60°-70° for 2 hours
- filtrationThe reaction mixture was filtered
- washthe separated solids were washed with methanol
- customthe combined organic solutions were evaporated to dryness
- customThe residue was purified by medium pressure liquid chromatography on silica
- washeluting with chloroform