反应详情

温度

160 °C

A solution of 4,4'-dinitro-2-biphenylamine (12.00 g, 46.29 mmol), 4-dimethylaminopyridine (5.77 g, 47.22 mmol) and N-methyl-2-pyrrolidinone (130ml) was stirred under a nitrogen atmosphere. Benzoyl chloride (9.69 g, 68.92 mmol) was added by dropping funnel at ambient temperature and the mixture heated to 160° C. and maintained at that temperature for 18 h. The resulting solution was poured into 1200 ml ice water with stirring and continued stirring overnight to give a light brown precipitate. The precipitate was filtered out and washed with water (2×100 ml), 5% sodium bicarbonate solution (2×100 ml) and water (4×200 ml) until the filtrate was clear. The crude product was dried under reduced pressure at 138° C. for 24 h to give 4,4'-dinitrobiphenyl-2-benzamide as a light brown powder (16.65 g, 99%), m.p. 242°-244° C.

1. customat ambient temperature
2. temperaturemaintained at that temperature for 18 h
3. stirringcontinued stirring overnight
4. customto give a light brown precipitate
5. filtrationThe precipitate was filtered out
6. washwashed with water (2×100 ml), 5% sodium bicarbonate solution (2×100 ml) and water (4×200 ml) until the filtrate
7. dry with materialThe crude product was dried under reduced pressure at 138° C. for 24 h