HRID2389969
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
- 46 °C
PROCEDURE
实验过程
To a suspension of NaH (120 mg, 5.00 mmol) in DMF (15 mL) was added 6-bromo-4-methyl-2-(methylthio)pyrido[2,3-d]pyrimidin-7(8H)-one (572 mg, 2 mmol). The mixture was heated to 46° C. The solution was cooled down slightly and 2-iodopropane (0.30 mL, 3.0 mmol) was added. The mixture was heated at 46° C. for 30 min and then cooled to room temperature and partitioned between water and ethyl acetate. The organic phase was dried (MgSO4) and concentrated. The crude product was purified by silica gel flash chromatography, using EtOAc/Hexane, to give the title compound (390 mg, 59%).
WORKUP
后处理
- temperatureThe solution was cooled down slightly
- temperatureThe mixture was heated at 46° C. for 30 min
- temperaturecooled to room temperature
- custompartitioned between water and ethyl acetate
- dry with materialThe organic phase was dried (MgSO4)
- concentrationconcentrated
- customThe crude product was purified by silica gel flash chromatography