반응 #649755

반응 방정식

2-methyl-5-nitrophenylguanidine nitrate

3-dimethylamino-1-(3-pyridyl)-2-propen-1-one

sodium hydroxide

→

N-(2-methyl-5-nitrophenyl)-4-(3-pyridyl)-2-pyrimidine-amine

용매

isopropanol

반응 조건

후처리

1. 1
   온도at reflux for 12 hours
2. 2
   여과filtration
3. 3
   세척washing with 2.0 liters of isopropanol and 3.times
4. 4
   건조400 ml of methanol and drying

실험 절차

248.2 g (0.96 mol) of 2-methyl-5-nitrophenylguanidine nitrate are added to a solution of 170 g (0.96 mol) of 3-dimethylamino-1-(3-pyridyl)-2-propen-1-one in 2.0 liters of isopropanol. After the addition of 42.5 g of sodium hydroxide, the reddish suspension is boiled at reflux for 12 hours. After cooling to 0° C., filtration, washing with 2.0 liters of isopropanol and 3.times.400 ml of methanol and drying, there is obtained N-(2-methyl-5-nitrophenyl)-4-(3-pyridyl)-2-pyrimidine-amine, m.p. 195° C.-198° C., Rf=0.68 (methylene chloride:methanol=9.1).

출처