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

HRID 81092

Reaktionsgleichung

Reaktionsgleichung von HRID 81092
[Cl:1][C:2]1[CH:7]=[C:6]([NH2:8])[CH:5]=[C:4]([Cl:9])[N:3]=1.[N+:10]([O-])([OH:12])=[O:11]>S(=O)(=O)(O)O>[Cl:1][C:2]1[CH:7]=[C:6]([NH:8][N+:10]([O-:12])=[O:11])[CH:5]=[C:4]([Cl:9])[N:3]=1

Komponenten

4

Edukt 2

HCID 944Nitric AcidHCID 1376524-Amino-2,6-dichloropyridine

Produkt 1

HCID 4216172,6-Dichloro-4-nitraminopyridine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1118Sulfuric AcidLösungsmittel

Versuchsvorschrift

A solution of 2,6-dichloropyridin-4-amine (500 g, 3.08 mol) in sulfuric acid (5 L) was cooled to 0° C. Nitric acid (2 L, 15 mol) was slowly added dropwise to the above resulting solution. The starting 2,6-dichloropyridin-4-amine was consumed after 3 hr. The reaction mixture was added to water (20 L), and the solid was filtered to give N-(2,6-dichloropyridin-4-yl)nitramide. This material was used directly in the next step. 1H NMR (CDCl3, 400 MHz): δ 7.11-7.14 (m, 1H), 7.09-7.09 (s, 1H).

Aufarbeitung

  1. customThe starting 2,6-dichloropyridin-4-amine was consumed after 3 hr
  2. additionThe reaction mixture was added to water (20 L)
  3. filtrationthe solid was filtered

Quellen und Nachweise

ORD-Eintrag
ord-7ed9d536285345c995d323239fc16bbc
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08846657B2

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