反应详情

2-Amino-4-chloro-6-methylamino-1,3,5-triazine (0.2 mole) was slurried in 80 ml of 2,2,2-trifluoroethanol at room temperature. Potassium hydroxide pellets (0.2 mole) were added portionwise and the mixture was stirred at room temperature overnight. The following day the reaction was heated at gentle reflux for 2 hours during which time the solids gradually dissolved. The solution was cooled and the solvent was removed under vacuum. The residue was washed with water and filtered to give 20.9 g shining off-white crystals of the product named above with the following characteristics: m.p. 204°-205° C. NMR (DMSO-d6): δ2.75, d, (NHCH3); 4.8, q, (OCH2CF3); 6.5-7.3, m, (NH2 +NHCH3).

1. temperatureThe following day the reaction was heated
2. temperatureat gentle reflux for 2 hours during which time the solids
3. dissolutiongradually dissolved
4. temperatureThe solution was cooled
5. customthe solvent was removed under vacuum
6. washThe residue was washed with water
7. filtrationfiltered
8. customto give 20.9 g