HRID7498
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
The starting material 2-fluoro-5-hydroxy-4-methylnitrobenzene, was obtained by adding 2M aqueous sodium hydroxide solution (13.1 ml), dropwise, to a solution of 2-fluoro-5-methoxycarbonyloxy-4-methylnitrobenzene (6 g, 26 mmol), (prepared as described in European Patent Publication No. 307777), in methanol (70 ml) cooled at 0° C. After stirring for 30 minutes, the mixture was concentrated by evaporation. After dilution with water, the solution was adjusted to pH2 and extracted with ethyl acetate. The organic layer was washed with water and then brine, dried (MgSO4) and the solvent evaporated to give 2-fluoro-5-hydroxy-4-methylnitrobenzene as a yellow solid (4 g, 90%).
WORKUP
后处理
- concentrationthe mixture was concentrated by evaporation
- extractionextracted with ethyl acetate
- washThe organic layer was washed with water
- dry with materialbrine, dried (MgSO4)
- customthe solvent evaporated