HRID37163

反应详情

EQUATION

反应方程式

HRID 37163 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. stirringAfter being stirred for 4 hours at room temperature
  2. concentrationthe reaction mixture is concentrated under reduced pressure
  3. extractionextracted with methylene chloride
  4. concentrationAfter the methylene chloride phases have been concentrated to dryness
  5. customthe crude product is purified by chromatography on a silica column (eluant:petroleum ether/ethyl acetate, 80:20)