反应详情

温度

120 °C

Phosphorus oxychloride (220.7 g) was added to isonicotinic acid N-oxide (50.064 g), and the mixture was stirred on an oil bath at 120° C. for 7 hours. The reaction mixture was slowly poured into ice water with vigorously stirring to precipitate light yellow crystals. The mixture was adjusted to approximately pH 4 with 4N NaOH aqueous solution. The resulting crystals were filtered out, washed with water, and dried by vacuum heating (60° C.) to obtain the above-captioned compound ([9]-(92)-467) (37.845 g).

1. stirringwith vigorously stirring
2. customto precipitate light yellow crystals
3. filtrationThe resulting crystals were filtered out
4. washwashed with water
5. customdried by vacuum
6. temperatureheating (60° C.)
7. customto obtain the above-captioned compound ([9]-(92)-467) (37.845 g)