反应详情

A mixture of 11.5 g (0.037 mole) of [2-[(3-amino-2-pyridinyl)amino]phenyl](4-fluorophenyl)methanone and 0.6 g of para toluene sulfonic acid in toluene was refluxed for 24 hr using a Dean-Stark trap to collect water. At the end of reflux, some of the toluene (300 ml) was distilled off and the hot solution was filtered. Pet.-ether (30°-60°) was added to cloud point. The solution was refrigerated overnight (0° C.) and filtered to give 10.7 g crystals. A portion of the material was recrystallized from isopropyl alcohol and dried in vacuo overnight at 65° C., m.p. 203°-205° C.

1. temperaturewas refluxed for 24 hr
2. customto collect water
3. temperatureAt the end of reflux
4. distillationsome of the toluene (300 ml) was distilled off
5. filtrationthe hot solution was filtered
6. addition-ether (30°-60°) was added to cloud point
7. filtration(0° C.) and filtered