反应详情

To 15 g (0.069 mole) of 5-bromo-2-hydroxy nicotinic acid was added 75 ml of thionyl chloride and 3 ml of dimethylformamide. The mixture was heated to reflux for 30 minutes. After cooling, the excess thionyl chloride was removed by rotary evaporation and the residue poured into water (1 liter) with vigorous agitation. The precipitate was collected and the mother liquor condensed to 1/2 the volume, yielding additional precipitate. The precipitates were combined and crystallized from toluene giving 6 g (37%) of material. The product was recrystallized from toluene, m.p. 174°-177° C.

1. temperatureThe mixture was heated
2. temperatureto reflux for 30 minutes
3. temperatureAfter cooling
4. customthe excess thionyl chloride was removed by rotary evaporation
5. additionthe residue poured into water (1 liter) with vigorous agitation
6. customThe precipitate was collected
7. customthe mother liquor condensed to 1/2 the volume
8. customyielding additional precipitate
9. customcrystallized from toluene giving 6 g (37%) of material
10. customThe product was recrystallized from toluene, m.p. 174°-177° C.