反应详情

温度

185 °C

3.3 g. (9.6 mmole) of 2-chloro-4,6-di(2,3,3-trimethyl-2-butyl)amino-s-triazine and 3.3 g. (30 mmoles) of 2,3,3-trimethyl-2-butylamine are heated at reflux (oil bath 185° C.) for 21 hours. Thin layer chromatography of a sample of the reaction mixture indicates a mixture of starting material and product in a ratio of 3:7. Heating is terminated and the reaction mixture is treated with excess aqueous NaOH. Filtration affords a 4.9 g. of crude beige product. This is digested with 15 ml. of hot acetone, filtered and 2.6 g. of beige solid collected, m.p. 278° C. dec. Recrystallization of this product from hot ethanol gives the pure product, m.p. 317°-321° C. dec.

1. additiona mixture of starting material and product in a ratio of 3:7
2. temperatureHeating
3. customis terminated
4. additionthe reaction mixture is treated with excess aqueous NaOH
5. filtrationFiltration
6. customaffords a 4.9 g
7. filtrationof hot acetone, filtered
8. customof beige solid collected
9. customRecrystallization of this product from hot ethanol
10. customgives the pure product, m.p. 317°-321° C. dec.