反应详情

温度

180 °C

A stirred mixture of 23.2 g (0.1 mole) of 2-amino-4'-chlorobenzophenone and 14.2 g (0.11 mole) of 3-amino-2-chloropyridine was heated at 180° C. under nitrogen atmosphere for 2.5 hr. The mixture solidified upon cooling to room temperature and was broken up with a spatula. The solid was suspended in 100 ml of methylene chloride and collected by filtration. The filter cake was dissolved in a mixture of water-methanol, basified with 3N sodium hydroxide and extracted twice with methylene chloride. The combined methylene chloride extracts were dried over magnesium sulfate and evaporated under reduced pressure. The residue which had crystallized was triturated in isopropyl ether and the solid (16.7 g) collected by filtration. A 3 g sample was recrystallized from isopropyl ether to give 1.6 g product; m.p. 153°-155° C.

1. temperatureupon cooling to room temperature
2. filtrationcollected by filtration
3. dissolutionThe filter cake was dissolved in a mixture of water-methanol
4. extractionextracted twice with methylene chloride
5. dry with materialThe combined methylene chloride extracts were dried over magnesium sulfate
6. customevaporated under reduced pressure
7. customThe residue which had crystallized
8. customwas triturated in isopropyl ether
9. filtrationthe solid (16.7 g) collected by filtration
10. customA 3 g sample was recrystallized from isopropyl ether