反应详情

The portion (4.56 g) was dissolved in 50 mL of ethanol, 1.72 g of thiourea was added to the solution, and the mixture was heated to reflux for 1 hour. Next, to the reaction solution added 20 mL of ethanol and the solution was cooled, and further 4.79 g of N-[4-(2,2-dicyanovinyl)phenyl]acetamide and 3 g of sodium bicarbonate were added thereto, and then the mixture was heated to reflux for 1.5 hours. After the reaction solution was allowed to cool, 2.02 g of NBS was added to the solution, and the mixture was heated to reflux for 30 minutes. After reaction solution was allowed to cool, furthermore diisopropyl ether was added thereto, and the inorganic material precipitated was filtrated off, then the filtrate was again concentrated and dissolved in ethanol. Saturated aqueous sodium bicarbonate was added to the solution and the resulting crystal was filtrated, washed with water and ethanol, and then dried under reduced pressure to give 3.2 g of N-{4-[6-amino-5-cyano-2-(6-methylpyridin-2-ylmethylsulfanyl)pyrimidin-4-yl]phenyl}acetamide as a white powder.

1. temperaturethe mixture was heated
2. temperatureto reflux for 1 hour
3. temperaturethe solution was cooled
4. temperaturethe mixture was heated
5. temperatureto reflux for 1.5 hours
6. temperatureto cool
7. temperaturethe mixture was heated
8. temperatureto reflux for 30 minutes
9. customAfter reaction solution
10. temperatureto cool
11. customthe inorganic material precipitated
12. filtrationwas filtrated off
13. concentrationthe filtrate was again concentrated
14. dissolutiondissolved in ethanol
15. additionSaturated aqueous sodium bicarbonate was added to the solution
16. filtrationthe resulting crystal was filtrated
17. washwashed with water and ethanol
18. customdried under reduced pressure