反应详情

温度

80 °C

A solution of 3-(3,5-dibromobenzoyl)pyridine (Preparation 1; 19.0 g) and hydrazine hydrate (13.9 ml) in ethylene glycol (140 ml) was heated under reflux for 45 minutes. The volatile material was distilled off until the internal temperature reached 180° C, and then the reaction mixture was cooled to 80° C. Potassium hydroxide (7.80 g) was added and the resulting solution was heated under reflux for 30 minutes, cooled and then poured into water. The mixture was extracted several times with ethyl acetate, and the combined extracts were washed with water and dried (MgSO4). Evaporation under vacuum gave the title compound (16.38 g), m.p. 70°-72° C. (after crystallisation from ethyl acetate-hexane). Found: C, 44.29; H, 2.66; N, 4.29. C12H9 Br2N requires C, 44.07; H, 2.77; N, 4.28%.

1. temperatureunder reflux for 45 minutes
2. distillationThe volatile material was distilled off until the internal temperature
3. customreached 180° C
4. additionPotassium hydroxide (7.80 g) was added
5. temperaturethe resulting solution was heated
6. temperatureunder reflux for 30 minutes
7. temperaturecooled
8. additionpoured into water
9. extractionThe mixture was extracted several times with ethyl acetate
10. washthe combined extracts were washed with water
11. dry with materialdried (MgSO4)
12. customEvaporation under vacuum
13. customgave
14. customthe title compound (16.38 g), m.p. 70°-72° C. (after crystallisation from ethyl acetate-hexane)