反应详情

A mixture containing 10.0 g (38.9 mmoles) of 4-chloro-2,6-bis(1,1-dimethylethylamino)pyrimidine, 13.42 g (155.8 mmoles) of piperazine and 150 ml of N-ethylmorpholine is boiled under reflux under nitrogen for 25 hours, then the solvent and piperazine are distilled off under atmospheric pressure. Water is added to the residue and distilled off until the head temperature reaches 100° C. After cooling down the residue is distributed between 200 ml of chloroform and 30 ml of 10% sodium hydroxide solution. After separation the organic phase is washed 4 times with 50 ml of water each, then dried and evaporated. The residue is purified by chromatography on a silica gel column by using a 9:1 mixture of chloroform and methanol. After recrystallizing the eluted product from hexane, the title compound is obtained in a yield of 7.65 g (64%), m.p.:142°-145° C.

1. temperatureunder reflux under nitrogen for 25 hours
2. distillationthe solvent and piperazine are distilled off under atmospheric pressure
3. additionWater is added to the residue
4. distillationdistilled off until the head temperature
5. customreaches 100° C
6. temperatureAfter cooling down the residue
7. customAfter separation the organic phase
8. washis washed 4 times with 50 ml of water each,
9. customthen dried
10. customevaporated
11. customThe residue is purified by chromatography on a silica gel column
12. additiona 9:1 mixture of chloroform and methanol
13. customAfter recrystallizing the eluted product from hexane