反应详情

A mixture containing 9.58 g (34.7 mmoles) of 4-chloro-2,6-bis(1,1-dimethylethylamino)pyrimidine, 11.95 g (138.8 mmoles) of piperazine and 150 ml of N-ethylmorpholine is boiled under reflux and nitrogen atmosphere for 25 hours, then the solvent and the excess of piperazine are distilled off under atmospheric pressure. Subsequently, 100 ml of water are added to the residue and the distillation is continued 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/methanol as eluent. After evaporating the eluate the residue is recrystallized from hexane to obtain the title compound in a yield of 64%, m.p.: 142°-145° C.

1. temperatureunder reflux
2. distillationthe solvent and the excess of piperazine are distilled off under atmospheric pressure
3. additionSubsequently, 100 ml of water are added to the residue
4. distillationthe distillation
5. customreaches 100° C
6. temperatureAfter cooling down
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/methanol as eluent
13. customAfter evaporating the eluate the residue
14. customis recrystallized from hexane