反应详情

Hydrogen chloride was bubbled through cold octanol (25 g, 190 mmol) until a weight gain of 4.2 g had registered. Nicotinic acid N-oxide (5.29 g, 38 mmol) was then added and the resulting mixture was stirred and heated at 95°-100° C. for 3 hours and 40 minutes. The excess octanol was then removed by distillation at reduced pressure, and the residue of the distillation was taken up in dichloromethane. The dichloromethane solution was washed with aqueous sodium bicarbonate and then with water, dried over anhydrous magnesium sulfate, filtered and evaporated under reduced pressure. The residue was recrystallized from ligroine to give 7.73 g (31 mmol) of octyl nicotinate N-oxide, mp 69.5°-71° C.

1. temperatureheated at 95°-100° C. for 3 hours and 40 minutes
2. customThe excess octanol was then removed by distillation at reduced pressure
3. distillationthe residue of the distillation
4. washThe dichloromethane solution was washed with aqueous sodium bicarbonate
5. dry with materialwith water, dried over anhydrous magnesium sulfate
6. filtrationfiltered
7. customevaporated under reduced pressure
8. customThe residue was recrystallized from ligroine