反应详情

A suspension of 6.6 g (0.02 mole) of [2-[(3-amino-2-pyridyl)amino]-4-chlorophenyl]-(phenyl)methanone (Intermediate 2) in 200 ml of toluene was heated at reflux over night under nitrogen atmosphere. The reaction mixture was filtered hot and the filtrate heated back to reflux temperature. The precipitate formed in cooling to room temperature was separated by filtration and recrystallized from benzene and dried 4 hr at 97°-98° C./0.1 mm Hg and over night at room temperature/0.1 mm Hg to give 3.7 g; m.p. 250.5° to 252° C. Elemental analysis for carbon was high and the product was redried at 139° C. (xylenes in drying pistol) for 8 hr. Although the carbon analysis remained high, the proton nuclear magnetic resonance spectrum and mass spectrum was consistent with the proposed structure.

1. temperaturewas heated
2. temperatureat reflux over night under nitrogen atmosphere
3. filtrationThe reaction mixture was filtered hot
4. temperaturethe filtrate heated back
5. temperatureto reflux temperature
6. customThe precipitate formed
7. customwas separated by filtration
8. customrecrystallized from benzene
9. customdried 4 hr at 97°-98° C./0.1 mm Hg
10. customover night at room temperature/0.1 mm Hg to give 3.7 g
11. customthe product was redried at 139° C.
12. dry with material(xylenes in drying pistol) for 8 hr