HRID2401471
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
CONDITIONS
反应条件
- 温度
- 60 °C
PROCEDURE
实验过程
To a solution of the crude 3-hydroxy-2-methyl-4-nitrobenzoic acid in acetone (300 mL) was added K2CO3 (15.8 g, 115 mmol) and Me2SO4 (8.7 g, 69 mmol). The mixture was refluxed at 60° C. for 2 h. After the solvent was evaporated in vacuo, the resulting residue was purified by silica gel-column (eluting with PE/EA=10:1) to afford methyl 3-methoxy-2-methyl-4-nitrobenzoate as a yellowish solid (2.7 g, 33% yield, two steps). m/z (ES+APCI)+: [M+H]+226.1.
WORKUP
后处理
- customAfter the solvent was evaporated in vacuo
- customthe resulting residue was purified by silica gel-column (eluting with PE/EA=10:1)