反应 #2328437

反应方程式

5-bromo-2-chloro-3-methylpyrimidin-4(3H)-one

4-fluorobenzenamine

NaHCO3

→

desired product

收率 99.0%

5-bromo-2-(4-fluorophenylamino)-3-methylpyrimidin-4(3H)-one

收率 99.0%

溶剂

n-BuOH

EtOAc

反应条件

后处理

1. 1
   其他prepared
2. 2
   温度The reaction mixture was cooled to room temperature
3. 3
   洗涤The EtOAc layer washed with H2O and saturated aqueous NaCl
4. 4
   萃取The aqueous phase was re-extracted with EtOAc
5. 5
   干燥The combined EtOAc layers were dried (Na2SO4)
6. 6
   过滤filtered
7. 7
   浓缩concentrated

实验过程

A mixture of 5-bromo-2-chloro-3-methylpyrimidin-4(3H)-one (0.100 g, 0.448 mmol; prepared according to the procedure of Example 46, Step B), 4-fluorobenzenamine (0.056 ml, 0.582 mmol) and NaHCO3 (0.150 g, 1.79 mmol) in n-BuOH (3 mL) was stirred at 60° C. overnight. The reaction mixture was cooled to room temperature and then diluted with EtOAc. The EtOAc layer washed with H2O and saturated aqueous NaCl. The aqueous phase was re-extracted with EtOAc. The combined EtOAc layers were dried (Na2SO4), filtered and concentrated to yield the desired product (0.132 g, 99%) as a pale yellow solid that was used without further purification.

来源