HRID1443453
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
To a solution of 2-amino-4-methoxy-3-methyl benzoic acid (3.1 g, 17.1 mmol) in dry DMF (40 ml) was added potassium carbonate (2.4 g, 17.1 mmol) and the mixture was stirred at room temperature for 30 minutes. Methyl iodide (3.1 g, 22 mmol) was added and the mixture was stirred for three hours at room temperature. A 5% aqueous solution of citric acid was added and the mixture was extracted three times with ethyl acetate. The organic phase was washed with water, dried with sodium sulfate and evaporated under reduced pressure. The product was isolated by column chromatography on silica gel eluted with hexane-ethyl acetate which gave the title compound (2.75 g).
WORKUP
后处理
- stirringthe mixture was stirred for three hours at room temperature
- extractionthe mixture was extracted three times with ethyl acetate
- washThe organic phase was washed with water
- dry with materialdried with sodium sulfate
- customevaporated under reduced pressure
- customThe product was isolated by column chromatography on silica gel
- washeluted with hexane-ethyl acetate which