反应详情

温度

10 °C

A 21 g. portion of piperazine in 500 ml. of methyl cellosolve is treated with 17.1 g. of 2-chloro-4,6-bis[(1,1,2,2-tetramethylpropyl)amino]-s-triazine. The mixture is stirred at reflux for 8 hours and then at room temperature. The mixture is filtered and the filtrate is taken to dryness in vacuo. The residue is shaken with 200 ml. of water, filtered, the insolubles collected, washed with 500 ml. of water and dried. The solid is suspended in 500 ml. of boiling ethanol, 150 ml. of methyl cellosolve is added and the mixture is concentrated to 300 ml., clarified and cooled to 10° C. The mixture is then taken to dryness in vacuo and the residue is recrystallized from 250 ml. of 60% ethanol with charcoal. The solid is washed with 100 ml. of 50% cold ethanol and dried giving the desired product, m.p. 183°-185° C.

1. temperatureat reflux for 8 hours
2. customat room temperature
3. filtrationThe mixture is filtered
4. stirringThe residue is shaken with 200 ml
5. filtrationof water, filtered
6. customthe insolubles collected
7. washwashed with 500 ml
8. dry with materialof water and dried
9. additionof methyl cellosolve is added
10. concentrationthe mixture is concentrated to 300 ml
11. customthe residue is recrystallized from 250 ml
12. washThe solid is washed with 100 ml
13. dry with materialof 50% cold ethanol and dried