Hydrochloric Acid → HCID 178526838, Verbindung

Temperatur

53 °C

Concentrated hydrochloric acid (239 g) was added to 2-hydroxy-5-nitropyridine (40.0 g). The resulting slurry was heated to 53° C., and stirred until all the solids dissolved. To this was slowly added a solution of potassium chlorate (14.0 g) in water (250 g), while maintaining the temperature between 55° C. and 59° C. The resulting mixture was stirred at 58–62° C. for about 1 hour. The reaction was then cooled to room temperature, stirred for 12 hours and then filtered. After washing the wet cake with water, the product was dried in a vacuum oven. 1H NMR (400 MHz/DMSO-d6) δ 8.64 (d, J=2.9 Hz, 1H), 8.35 (d, J=2.9 Hz, 1H)

1. dissolutiondissolved
2. temperaturewhile maintaining the temperature between 55° C. and 59° C
3. stirringThe resulting mixture was stirred at 58–62° C. for about 1 hour
4. temperatureThe reaction was then cooled to room temperature
5. stirringstirred for 12 hours
6. filtrationfiltered
7. washAfter washing the wet cake with water
8. customthe product was dried in a vacuum oven

ORD-Eintrag

ord-79a75d3a07254c3fadee3dd8f37571b9

Quelldatensatz

uspto-grants-2008_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07351833B2