HRID323397

反应详情

EQUATION

反应方程式

HRID 323397 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Combine methyl 3-methoxy-4,5-dihydroxybenzoate (0.93 g, 4.6 mmol) and potassium carbonate (3.2 g, 23.4 mmol) in acetone (25 mL) and dimethylformamide (25 mL). Add diiodomethane (6.3 g, 23.3 mmol). Heat to reflux. After 24 hours, cool in an ice bath, acidify with a 1 M aqueous hydrochloric acid solution (35 mL), and extract twice with ethyl acetate. Combine the organic layers and extract with brine. Dry over MgSO4, filter, and concentrate in vacuo to give methyl 3-methoxy-4,5-methylenedioxybenzoate.

WORKUP

后处理

  1. temperatureHeat to reflux
  2. temperaturecool in an ice bath
  3. extractionextract twice with ethyl acetate
  4. extractionextract with brine
  5. dry with materialDry over MgSO4
  6. filtrationfilter
  7. concentrationconcentrate in vacuo