Diethylamine → N,N-Diethyl-2-methyl-5-nitropyridine-3-carboxamide

HRID 972753Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 972753
[CH3:1][C:2]1[N:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:3]=1[C:4]([OH:6])=O.[CH2:14]([NH:16][CH2:17][CH3:18])[CH3:15]>C(Cl)(Cl)Cl>[CH2:14]([N:16]([CH2:17][CH3:18])[C:4](=[O:6])[C:3]1[CH:7]=[C:8]([N+:11]([O-:13])=[O:12])[CH:9]=[N:10][C:2]=1[CH3:1])[CH3:15]

Komponenten

4

Edukt 2

HCID 8021DiethylamineHCID 2872402-Methyl-5-nitropyridine-3-carboxylic acid

Produkt 1

HCID 21405249N,N-Diethyl-2-methyl-5-nitropyridine-3-carboxamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Versuchsvorschrift

In dry chloroform were dissolved 0.3 g of 2-methyl-5-nitronicotinic acid and 1.5 ml of diethylamine. After addition of 10 g of phosphorous pentaoxide, the mixture was stirred with heating at 55° - 60° C. for 3 hours. After cooling, the chloroform portion was separated and evaporated under reduced pressure. The residue was, after addition of water, neutralized with sodium hydrogen carbonate and extracted with ethyl acetate. The extract was concentrated and purified on a silica gel column to give 0.25 g of a colorless oil.

Aufarbeitung

  1. additionAfter addition of 10 g of phosphorous pentaoxide
  2. temperaturewith heating at 55° - 60° C. for 3 hours
  3. temperatureAfter cooling
  4. customthe chloroform portion was separated
  5. customevaporated under reduced pressure
  6. additionafter addition of water
  7. extractionextracted with ethyl acetate
  8. concentrationThe extract was concentrated
  9. custompurified on a silica gel column

Quellen und Nachweise

ORD-Eintrag
ord-d7b2854d4e034bd0b0ed3318118488d7
Quelldatensatz
uspto-grants-1977_10
Patentnummer
US04053608

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