反应 #51438

反应方程式

acetylchloride

( 2 )

(3-chloro-4-fluorophenyl)-(2,6-dichloro-7,8-dihydropyrimido[5,4-d]pyrimidin-4-yl)amine

N-ethyldiisopropylamine

→

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

溶剂

ethyl acetate

反应条件

后处理

1. 1
   洗涤washed 3 times with 700 ml of water at 60° C
2. 2
   其他The organic phase is evaporated down
3. 3
   温度cooled to 0-5° C.
4. 4
   workup.STIRRINGstirred at this temperature for 30 minutes
5. 5
   其他The product that crystallises out
6. 6
   过滤is filtered off
7. 7
   其他dried at 60° C. in vacuo

实验过程

At 10° C., 56.4 ml (0.789 mol) of acetylchloride are added dropwise to a suspension of 210.6 g (0.608 mol) of (2) and 176 ml of N-ethyldiisopropylamine (0.95 mol) in 2.1 l of ethyl acetate. The mixture is stirred for 90 minutes at ambient temperature and then washed 3 times with 700 ml of water at 60° C. The organic phase is evaporated down and combined with 590 ml of ethanol. The mixture is briefly brought to boiling point, cooled to 0-5° C. and stirred at this temperature for 30 minutes. The product that crystallises out is filtered off and dried at 60° C. in vacuo. Yield: 180.3 g (76.3%), melting point: 177.6° C.

来源