反应详情

54.9 g (0.96 mole) of allylamine are added dropwise, in the course of 1.5 hours and while stirring, to a clear solution of 73.8 g (0.4 mole) of cyanuric chloride in 500 ml of toluene, the temperature being kept between 20° and 30° by applying gentle external cooling to the reaction vessel. After stirring for a further two hours at room temperature and for one hour at 50°, the mixture is cooled to 20°, and a solution of 16 g (0.4 mole) of sodium hydroxide in 70 ml of water is added dropwise at 20° in the course of 2 hours. After stirring for a further 2 hours at room temperature and for 6 hours at 60°, a further 16 g (0.4 mole) of sodium hydroxide in 70 ml of water are added dropwise in the course of 2 hours and stirring is continued for a further 5 hours at 60°. After the mixture has cooled to room temperature, 200 ml of water are added, and the precipitate is filtered off after stirring for approx. 30 minutes. The precipitate is thoroughly washed with water, thoroughly suction-drained and dried in vacuo at approx. 95°. The colourless 2,4-bis-allylamino-6-chloro-1,3,5-triazine thus obtained is analytically pure and has a melting point of 205°-206°; its water content is <0.3%. Yield 88.2 g (97.7% of theory).

1. custombeing kept between 20° and 30°
2. temperatureby applying gentle external cooling to the reaction vessel
3. temperaturethe mixture is cooled to 20°
4. stirringAfter stirring for a further 2 hours at room temperature and for 6 hours at 60°
5. stirringstirring
6. waitis continued for a further 5 hours at 60°
7. temperatureAfter the mixture has cooled to room temperature
8. filtrationthe precipitate is filtered off
9. stirringafter stirring for approx. 30 minutes
10. washThe precipitate is thoroughly washed with water
11. customthoroughly suction-drained and dried in vacuo at approx. 95°