反应详情

A mixture of pyridine-3-sulphonic acid (3.0 g) and PCl5 (7.9 g) was stirred in an oil bath maintained at 150° for 3 hours, in a flask fitted with a reflux condenser. After cooling, the liquid formed set solid. The solid was triturated with xylene (10 cm3) and evaporated at the water pump in an oil-bath maintained at a maximum temperature of 110°, and with a splash-head to reduce frothing. The evaporation was repeated twice more, and the residue was pumped on a rotary evaporator to remove the last traces of xylene. The yellow, semi-crystalline mass (6.87 g) occluded unreacted PCl5.

1. temperaturemaintained at 150° for 3 hours, in a flask
2. customfitted with a reflux condenser
3. temperatureAfter cooling
4. customthe liquid formed
5. customThe solid was triturated with xylene (10 cm3)
6. customevaporated at the water pump in an oil-bath
7. temperaturemaintained at a maximum temperature of 110°
8. customThe evaporation
9. customthe residue was pumped on a rotary evaporator
10. customto remove the last traces of xylene