HRID1702602
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
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
- extractionextracted with ether
- washThe organic phase is washed with 10% potassium carbonate and saturated sodium chloride solution
- dry with materialdried over magnesium sulfate
- concentrationconcentrated
- customThe residue is chromatographed over silica gel with a 7:3 mixture of hexane/ether as eluant
- customaffording the compound of the formula ##STR5## with a refractive index of nD20° =1.5942