2-Chloro-3-nitropyridine → HCID 14677546, Verbindung

HRID 1084752Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1084752
Cl[C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[CH:4][N:3]=1.[CH3:11][C:12]1[CH:13]=[C:14]([CH2:17][NH2:18])[O:15][CH:16]=1.C(=O)([O-])O.[Na+]>C(O)C>[CH3:11][C:12]1[CH:13]=[C:14]([CH2:17][NH:18][C:2]2[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[CH:4][N:3]=2)[O:15][CH:16]=1

Komponenten

5

Edukt 3

HCID 796132-Chloro-3-nitropyridineHCID 516892Sodium BicarbonateHCID 146775454-Methyl-2-furanmethanamine

Produkt 1

HCID 14677546HCID 14677546, VerbindungAusbeute 91,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A mixture of 10.4 parts of 2-chloro-3-nitropyridine, 8 parts of 4-methyl-2-furanmethanamine, 7.6 parts of sodium hydrogen carbonate and 120 parts of ethanol was stirred overnight at reflux temperature. The reaction mixture was evaporated and the residue was taken up in water. The product was extracted with 1,1'-oxybisethane. The extract was dried, filtered and evaporated. The residue was purified by column chromatography over silica gel using trichloromethane as eluent. The pure fractions were collected and the eluent was evaporated, yielding 14.9 parts (91.2%) of N-[(4-methyl-2-furanyl)methyl]-3-nitro-2-pyridinamine as a residue (int. 3).

Aufarbeitung

  1. temperatureat reflux temperature
  2. customThe reaction mixture was evaporated
  3. extractionThe product was extracted with 1,1'-oxybisethane
  4. customThe extract was dried
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue was purified by column chromatography over silica gel
  8. customThe pure fractions were collected
  9. customthe eluent was evaporated

Quellen und Nachweise

ORD-Eintrag
ord-190f7989fd2f452d850880b0763e4e57
Quelldatensatz
uspto-grants-1991_04
Patentnummer
US05006527

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