Nitric Acid → 2,6-Dichloro-4-nitraminopyridine

Temperatur

-5 °C

2,6-dichloropyridine-4-ylamine (10.0 g, 61 mmol) was slowly added in concentrated sulfuric acid (64 mL) at the rate to keep the internal reaction temperature <10° C. The mixture was then cooled to −5° C. and nitric acid (90%, 30 mL) was added dropwise to keep the reaction temperature below 0° C. over a period of 40 minutes. The reaction mixture was stirred at 0° C. for 2 hours and then poured into ice-water (500 mL). The title compound was isolated by filtration and dried in vacuo for the next step.

1. customthe internal reaction temperature <10° C
2. customthe reaction temperature below 0° C.
3. customof 40 minutes

ORD-Eintrag

ord-dd246b41c86a40e2bcd278fecf4bee3a

Quelldatensatz

uspto-grants-2016_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09434726B2