反应详情

温度

100 °C

A reactor was charged with isopropyl 8-[(2,6-dimethylbenzyl)amino]-2,3-dimethylimidazo[1,2-a]pyridine-6-carboxylate (11.30 kg, 1 equiv., 27.02 mol) and THF (45 L), ethanolamine (18.97 kg, 11 equiv., 309.2 mol) was added at about 20° C. The suspension was heated to about 100° C. Some solvent was distilled off and then THF (35L) was added and the distillation was continued. The procedure of adding THF and distilling it off was repeated until complete conversion. To the suspension ethanol (140L) was added and the suspension was heated to reflux. To obtain a clear solution additional ethanol (13L) was added. The hot solution was filtered and then cooled. The white solid was filtered off, washed with ethanol and dried to yield the product as a white powder. (8271 g).

1. additionwas added at about 20° C
2. distillationSome solvent was distilled off
3. additionTHF (35L) was added
4. distillationthe distillation
5. distillationThe procedure of adding THF and distilling it
6. additionTo the suspension ethanol (140L) was added
7. temperaturethe suspension was heated to reflux
8. customTo obtain a clear solution additional ethanol (13L)
9. additionwas added
10. filtrationThe hot solution was filtered
11. temperaturecooled
12. filtrationThe white solid was filtered off
13. washwashed with ethanol
14. customdried