反应详情

温度

150 °C

Charge a 1 L auto-clave with 5-amino-4,6-dichloro-2-methylpyrimidine (50.0 g, 0.281 mol), 2-amino ethanol (18.8 g, 0.309 mol), diisopropylethylamine (54.5 g, 0.421 mol), and IPA (500 mL). Heat the mixture to 145-155° C., with stirring for 24 to 30 h. Cool the reaction to 25-30° C. Concentrate the reaction mixture, removing the solvent under vacuum below 50° C. Charge DCM (500 mL) into the mixture and stir at 10-25° C. for 2 h. Filter the mixture and dry the cake in the oven at 45-50° C. to give the product as a pale yellow solid (35.0 g). 1H NMR (dmso-d6): δ 6.76 (s, 1H); 4.79 (s, 3H); 3.53-3.37 (m, 4H); 2.09 (s, 3H).

1. temperatureCool
2. customthe reaction to 25-30° C
3. concentrationConcentrate the reaction mixture
4. customremoving the solvent under vacuum below 50° C
5. stirringCharge DCM (500 mL) into the mixture and stir at 10-25° C. for 2 h
6. filtrationFilter the mixture
7. customdry the cake in the oven at 45-50° C.