Diethylamine → HCID 20321213, Verbindung

HRID 866413Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 866413
[CH3:1][C:2]1[N:3]=[C:4]([N+:11]([O-:13])=[O:12])[CH:5]=[C:6]([CH:10]=1)[C:7]([OH:9])=O.[CH2:14]([NH:16][CH2:17][CH3:18])[CH3:15].O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O>C(Cl)(Cl)Cl>[CH2:14]([N:16]([CH2:17][CH3:18])[C:7](=[O:9])[C:6]1[CH:10]=[C:2]([CH3:1])[N:3]=[C:4]([N+:11]([O-:13])=[O:12])[CH:5]=1)[CH3:15]

Komponenten

5

Edukt 3

HCID 8021DiethylamineHCID 14812Phosphorus oxide (P4O10)HCID 124040282-Methyl-6-nitropyridine-4-carboxylic acid

Produkt 1

HCID 20321213HCID 20321213, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Versuchsvorschrift

To a mixture of 1.0 g. of 6-methyl-2-nitroisonicotinic acid, 20 ml. of chloroform and 3 ml. of diethylamine was added 7.0 g. of phosphorus pentoxide with stirring. The resulting mixture was refluxed for 1 hour. After cooling, the chloroform layer was separated and poured into 20 ml. of water. The resulting mixture was neutralized with sodium hydrogencarbonate and the chloroform layer was separated, dried over anhydrous sodium sulfate and the chloroform was distilled off in vacuo. The residual oil was gradually crystallized and then recrystallized from ethyl acetate-n-hexane to give 0.6 g. of the desired product.

Aufarbeitung

  1. additionTo a mixture of 1.0 g
  2. temperatureThe resulting mixture was refluxed for 1 hour
  3. temperatureAfter cooling
  4. customthe chloroform layer was separated
  5. additionpoured into 20 ml
  6. customthe chloroform layer was separated
  7. dry with materialdried over anhydrous sodium sulfate
  8. distillationthe chloroform was distilled off in vacuo
  9. customThe residual oil was gradually crystallized
  10. customrecrystallized from ethyl acetate-n-hexane
  11. customto give 0.6 g

Quellen und Nachweise

ORD-Eintrag
ord-3131f104a6e144bdbf284598435d6bbc
Quelldatensatz
uspto-grants-1978_07
Patentnummer
US04098893

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