反应详情

温度

110 °C

Under nitrogen atmosphere, 44.4 g (0.192 mole) of 2-amino-2'-chlorobenzophenone was added in four portions at 15 min intervals to a stirred melt (130°-135° C.) of 33.5 g (0.211 mole) of 2-chloro-3-nitropyridine. Heating was continued for 30 min at 130°-125° C. and for 45 min at 145° C. The reaction mixture was cooled to 110° C. and 200 ml of hot toluene was added. To the cooled mixture (room temperature) 100 ml of 10% aqueous sodium hydroxide was added and stirring was continued for 15 min. The toluene layer was separated and washed three times with 75 ml portions of water, dried over sodium sulfate and concentrated in vacuo. The residue was dissolved in 300 ml of methylene chloride and the solution was stirred with 100 g of fluorisil for 30 min. The mixture was filtered, rinsing the fluorisil filter-cake several times with methylene chloride. The combined filtrates were treated in the same manner with an additional 100 g of fluorisil. The methylene chloride was separated by filtration and concentrated in vacuo. The residue was crystallized from ethyl acetate-cyclohexane to give 26.0 g of a bright yellow solid, m.p. 119° C. A second crop (7.0 g) was obtained from the filtrate and recrystallized from isopropyl ether, m.p. 118°-119° C. The total yield amounted to 49% of theory.

1. temperatureHeating
2. waitwas continued for 15 min
3. customThe toluene layer was separated
4. washwashed three times with 75 ml portions of water
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated in vacuo
7. dissolutionThe residue was dissolved in 300 ml of methylene chloride
8. stirringthe solution was stirred with 100 g of fluorisil for 30 min
9. filtrationThe mixture was filtered
10. washrinsing the fluorisil
11. filtrationfilter-cake several times with methylene chloride
12. additionThe combined filtrates were treated in the same manner with an additional 100 g of fluorisil
13. customThe methylene chloride was separated by filtration
14. concentrationconcentrated in vacuo
15. customThe residue was crystallized from ethyl acetate-cyclohexane