HRID1433903
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
The title compound was synthesized by referring to Chem. Pharm. Bull., 1977, 25, 2788. To 3-methoxyphenol (8.5 g) and 3,3-dimethylacrylic acid (7.5 g) was added polyphosphoric acid (80 ml), and the solution was stirred for 2 hours at 100° C. The reaction mixture was poured into an ice water, the solution was stirred, and then extracted with diethyl ether, then sequentially washed with an aqueous solution of 2N sodium hydroxide, water and brine, dried over anhydrous magnesium sulfate, then filtered through NH silica gel, and the solvent was evaporated in vacuo. The residue was washed with a hexane-diethyl ether system to provide the title compound (10.6 g).
WORKUP
后处理
- customThe title compound was synthesized
- stirringthe solution was stirred
- extractionextracted with diethyl ether
- washsequentially washed with an aqueous solution of 2N sodium hydroxide, water and brine
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltered through NH silica gel
- customthe solvent was evaporated in vacuo
- washThe residue was washed with a hexane-diethyl ether system