反应 #51439

反应方程式

1-methyl-4-aminopiperidine

( 3 )

1-[2,6-Dichloro-8-(3-chloro-4-fluorophenylamino)-4H-pyrimido[5,4-d]pyrimidin-3-yl]ethanone

THF

triethylamine

→

1-[6-chloro-8-(3-chloro-4-fluorophenylamino)-2-(1-methylpiperidin-4-ylamino)-4H-pyrimido[5,4-d]pyrimidin-3yl]ethanone

溶剂

water

反应条件

后处理

1. 1
   workup.WAITIt is left
2. 2
   温度to cool to 40° C.
3. 3
   workup.STIRRINGthe mixture is then stirred for 90 minutes at 10° C
4. 4
   其他The product that crystallises out
5. 5
   过滤is filtered off
6. 6
   洗涤washed with 150 ml of water
7. 7
   其他dried in vacuo at 60° C
8. 8
   workup.DISSOLUTIONThe product is dissolved in 1150 ml of ethyl acetate
9. 9
   温度It is cooled to 10° C.
10. 10
    过滤filtered
11. 11
    其他the product that crystallises out
12. 12
    其他is dried at 60° C. in vacuo

实验过程

47.2 g (0.413 mol) of 1-methyl-4-aminopiperidine is added dropwise at ambient temperature to a mixture of 123.3 g (0.317 mol) of (3), 740 ml of THF and 61.7 ml (0.445 mol) of triethylamine. The mixture is stirred for 30 min at 50° C. It is left to cool to 40° C., 1480 ml of water are added and the mixture is then stirred for 90 minutes at 10° C. The product that crystallises out is filtered off, washed with 150 ml of water and dried in vacuo at 60° C. The product is dissolved in 1150 ml of ethyl acetate at boiling temperature. It is cooled to 10° C., filtered and the product that crystallises out is dried at 60° C. in vacuo. Yield: 128.9 g (87.2%).

来源