Reaktion #528050

Reaktionsgleichung

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

3-nitrophenylguanidine nitrate

sodium hydroxide

→

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

Lösungsmittel

isopropanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe yellow suspension is heated
2. 2
   Temperaturat reflux for 20 hours
3. 3
   Temperaturcooled to 0°
4. 4
   Filtrationfiltered
5. 5
   Waschenwashed with 30 ml of isopropanol
6. 6
   Filtrationfiltered
7. 7
   Waschenwashed with a small amount of cold ethanol

Vorschrift

1 g (5.68 mmol)of 3-dimethylamino-1-(2-pyridyl)-2-propen-1-one [EP-A-233 461] is dissolved in 8 ml of isopropanol, and 1.38 g (5.68 mmol) of 3-nitrophenylguanidine nitrate are added. After the addition of 0.25 g (6.24 mmol) of sodium hydroxide, the yellow suspension is heated at reflux for 20 hours, then cooled to 0°, filtered and washed with 30 ml of isopropanol. The filtration residue is stirred in 15 ml of ethanol for 20 minutes, filtered and washed with a small amount of cold ethanol, yielding N-(3-nitrophenyl)-4-(2-pyridyl)-2-pyrimidine-amine; m.p. 213°-219°.

Quelle