HRID390048
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
- 70 °C
PROCEDURE
实验过程
To a solution of 4-chloro-6-methyl-2-(methylthio)-5-pyrimidinecarbonitrile (500 mg, 2.51 mmol) in DMF (6 mL) were added 3-methylaniline (322 mg, 3.01 mmol) and diisopropyl ethylamine (712 mg, 5.52 mmol), and the reaction mixture was stirred 70° C. for 1.5 h. The mixture was cooled and concentrated, and the residue was dissolved into EtOAc (30 mL) and washed with water (10 mL). The ethyl acetate extract was dried over Na2SO4, filtered, and concentrated. The residue was purified using column chromatography (silica gel, hexane/EtOAc, 0 to 100%) to give the product (650 mg, 96% yield).
WORKUP
后处理
- temperatureThe mixture was cooled
- concentrationconcentrated
- dissolutionthe residue was dissolved into EtOAc (30 mL)
- washwashed with water (10 mL)
- extractionThe ethyl acetate extract
- dry with materialwas dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
- customThe residue was purified