HRID1513017
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 4,6-dichloro-2-methyl-5-nitropyrimidine (6.54 g) in methanol (31.5 mL) was added sodium methoxide (28% methanol solution, 6.05 mL) in a dropwise manner under ice-cooling, and the mixture was stirred at the same temperature for 1 hour, and then stirred at room temperature for 1.5 days. The reaction mixture was poured into water, and the resulting mixture was extracted with diethyl ether. The extract was washed with water and brine, and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure, and the residue was purified by column chromatography on silica gel (eluent: n-hexane−n-hexane/ethyl acetate=9/1) to give the title compound (5.7 g).
WORKUP
后处理
- temperaturecooling
- stirringstirred at room temperature for 1.5 days
- extractionthe resulting mixture was extracted with diethyl ether
- washThe extract was washed with water and brine
- dry with materialdried over anhydrous magnesium sulfate
- customThe solvent was removed under reduced pressure
- customthe residue was purified by column chromatography on silica gel (eluent: n-hexane−n-hexane/ethyl acetate=9/1)