反应详情

41.3 g (0.17 mol) of 3-nitrophenyl-guanidine nitrate, made into a slurry in 50 ml of isopropanol, are added to a solution of 30 g (0.17 mol) of 3-dimethylamino-1-(3-pyridyl)-2-propen-1-one [described in EP-A-0 233 461] in 250 ml of isopropanol. After the addition of 7.49 g (0.19 mol) of sodium hydroxide, the yellow suspension is boiled at reflux for 8 hours. After cooling to 0°, the mixture is filtered and washed with 200 ml of isopropanol. The filtration residue is made into a sherry in 300 ml of water and stirred for 30 minutes, filtered and washed with 200 ml of water. After again making into a slurry in 200 ml of ethanol and washing with 200 ml of ethanol/diethyl ether (1:1) there is obtained N-(3-nitrophenyl)-4-(3-pyridyl)-2-pyrimidine-amine; m.p. 212°-213° , Rf =0.75 (chlorofoform:menthol=9:1).

1. temperatureat reflux for 8 hours
2. temperatureAfter cooling to 0°
3. filtrationthe mixture is filtered
4. washwashed with 200 ml of isopropanol
5. filtrationfiltered
6. washwashed with 200 ml of water
7. washwashing with 200 ml of ethanol/diethyl ether (1:1) there