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
Stir for 15 minutes at room temperature, under argon, a solution of 0.48 mmol of methyl 6-hydroxy -1,4-benzodioxin-2-carboxylate in 5 cm3 of N,N-dimethylformamide in the presence of 0.57 mmol of 60% sodium hydride suspended in oil, and then add 0.72 mmol of methyl iodide. After being stirred for 4 hours at room temperature, the reaction mixture is concentrated under reduced pressure and then extracted with methylene chloride. After the methylene chloride phases have been concentrated to dryness, the crude product is purified by chromatography on a silica column (eluant:petroleum ether/ethyl acetate, 80:20). Methyl 6-methoxy -1,4-benzodioxin-2-carboxylate is thereby obtained in a yield of 78%.
WORKUP
后处理
- stirringAfter being stirred for 4 hours at room temperature
- concentrationthe reaction mixture is concentrated under reduced pressure
- extractionextracted with methylene chloride
- concentrationAfter the methylene chloride phases have been concentrated to dryness
- customthe crude product is purified by chromatography on a silica column (eluant:petroleum ether/ethyl acetate, 80:20)