反应详情

In 230 ml of N,N-dimethylformamide was dissolved 23.5 g of 4-dimethylamino-3-(imidazo[1,2-a]pyridin-6-yl)-3-buten-2-one. The solution was stirred at 80° to 90° C. for 12 hours, together with 9.48 g of α-cyanoacetamide and 12.2 g of sodium methoxide. After cooling, the solvent was removed by distillation under reduced pressure and 500 ml of water was added to the residue to dissolve it. The solution was washed with 600 ml of chloroform. Next, about 5 ml of acetic acid was added to the aqueous layer to adjust pH to 6.5. Crystals precipitated upon cooling were taken by filtration. After the crystals were washed with water, acetonitrile and then ether, they were dissolved in 200 ml of a 2.5% aqueous sodium hydroxide solution. The solution was treated with activated charcoal. The filtrate was again adjusted to pH of 6.5 with about 7 ml of acetic acid. Crystals precipitated upon cooling were taken by filtration. After the crystals were washed with water, acetonitrile and then ether, they were recrystallized from 100 ml of N,N-dimethylformamide to obtain 13 g of 1,2-dihydro-6-methyl-2-oxo-5-(imidazo[1,2-a]pyridin-6-yl)-3-pyridinecarbonitrile.

1. temperatureAfter cooling
2. customthe solvent was removed by distillation under reduced pressure and 500 ml of water
3. additionwas added to the residue
4. dissolutionto dissolve it
5. washThe solution was washed with 600 ml of chloroform
6. additionNext, about 5 ml of acetic acid was added to the aqueous layer
7. customCrystals precipitated
8. temperatureupon cooling
9. filtrationwere taken by filtration
10. washAfter the crystals were washed with water, acetonitrile
11. dissolutionether, they were dissolved in 200 ml of a 2.5% aqueous sodium hydroxide solution
12. additionThe solution was treated with activated charcoal
13. customCrystals precipitated
14. temperatureupon cooling
15. filtrationwere taken by filtration
16. washAfter the crystals were washed with water, acetonitrile
17. customether, they were recrystallized from 100 ml of N,N-dimethylformamide