HRID1702602

反应详情

EQUATION

反应方程式

HRID 1702602 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

10 g of α-ethynyl-3-phenoxybenzyl alcohol, 2.1 g of paraformaldehyde, 5.3 g of diisopropylamine, 0.215 g of CuBr and 50 ml of dioxane are refluxed for 2 hours. The reaction mixture is cooled to 20° C., poured into a solution of 2 N HCl and extracted with ether. The organic phase is washed with 10% potassium carbonate and saturated sodium chloride solution, dried over magnesium sulfate and concentrated. The residue is chromatographed over silica gel with a 7:3 mixture of hexane/ether as eluant, affording the compound of the formula ##STR5## with a refractive index of nD20° =1.5942.

WORKUP

后处理

  1. extractionextracted with ether
  2. washThe organic phase is washed with 10% potassium carbonate and saturated sodium chloride solution
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated
  5. customThe residue is chromatographed over silica gel with a 7:3 mixture of hexane/ether as eluant
  6. customaffording the compound of the formula ##STR5## with a refractive index of nD20° =1.5942