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
- 70 °C
PROCEDURE
实验过程
To a suspension of 5.9 g of 6-hydroxymethyl-5-hydroxy-2-methyl-4-pyrone in 60 ml of dimethylformamide were successively added 6.2 g of potassium carbonate and 6.2 ml of p-methoxybenzyl chloride. The mixture was stirred at 70° C. for 2 hours. The reaction liquid was concentrated and 200 ml of water and 400 ml of dichloromethane were added to the concentrate. The organic phase was then washed with 200 ml of water. After drying over anhydrous magnesium sulfate, the organic phase was concentrated under reduced pressure. The concentrate was then separated and purified by flash column chromatography (eluting solution; chloroform: methanol=20:1) using Wako Gel C-300 (300 g) to give 5.9 g of the title compound.
WORKUP
后处理
- customThe reaction liquid
- concentrationwas concentrated
- addition200 ml of water and 400 ml of dichloromethane were added to the concentrate
- washThe organic phase was then washed with 200 ml of water
- dry with materialAfter drying over anhydrous magnesium sulfate
- concentrationthe organic phase was concentrated under reduced pressure
- customThe concentrate was then separated
- custompurified by flash column chromatography (eluting solution; chloroform: methanol=20:1)