2-Chloro-5-nitropyridine → HCID 4418042, Verbindung

HRID 1030997Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1030997
Cl[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][N:3]=1>C(NCC)C.C(Cl)Cl>[CH2:2]([N:3]([CH2:4][CH3:5])[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][N:3]=1)[CH3:7]

Komponenten

4

Edukt 1

HCID 783082-Chloro-5-nitropyridine

Produkt 1

HCID 4418042HCID 4418042, VerbindungAusbeute 195,5 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6344DichloromethaneLösungsmittelHCID 8021DiethylamineLösungsmittel

Versuchsvorschrift

A stirred mixture of 27.6 g (0.174 mole) of 2-chloro-5-nitropyridine in 500 ml of diethylamine was heated at reflux for two days. The excess diethylamine was removed by distillation under reduced pressure, leaving a residue. This residue was dissolved in methylene chloride, and the organic solution was washed with an aqueous, 10% sodium hydroxide solution. The washed organic phase was dried over anhydrous magnesium sulfate and was filtered. The filtrate was evaporated under reduced pressure to yield 33.2 g of 2-diethylamino-5-nitropyridine as a solid. The nmr spectrum was consistent with the proposed structure.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureat reflux for two days
  3. customThe excess diethylamine was removed by distillation under reduced pressure
  4. customleaving a residue
  5. washthe organic solution was washed with an aqueous, 10% sodium hydroxide solution
  6. dry with materialThe washed organic phase was dried over anhydrous magnesium sulfate
  7. filtrationwas filtered
  8. customThe filtrate was evaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-ce5c4d0c44d6447eb50a8d7463a72ce8
Quelldatensatz
uspto-grants-1992_04
Patentnummer
US05108486

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