HRID1493359
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 solution of dimethyl 4-hydroxy-3-methyl-2,5-thiophene dicarboxylate (4.26 g) in acetone (100 ml) containing anhydrous potassium carbonate (2.34 g) was stirred for 1 hour at room temperature. Dimethyl sulphate (1.62 ml) was added and the solution refluxed for 2 hours. The solvent was then removed under vacuum and, after treating the residue with water-ethyl acetate, was extracted several times with ethyl acetate; the organic extracts were collected, washed with water, dried over anhydrous magnesium sulphate, filtered and the solvent evaporated to give a solid, m.p. 61°-64° ex methanol.
WORKUP
后处理
- temperaturethe solution refluxed for 2 hours
- customThe solvent was then removed under vacuum
- additionafter treating the residue with water-ethyl acetate
- extractionwas extracted several times with ethyl acetate
- customthe organic extracts were collected
- washwashed with water
- dry with materialdried over anhydrous magnesium sulphate
- filtrationfiltered
- customthe solvent evaporated
- customto give a solid, m.p. 61°-64° ex methanol