Chloroform → HCID 15614715, Verbindung

HRID 477648Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 477648
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][NH:9][C:10]2[CH:11]=[N:12][CH:13]=[CH:14][C:15]=2[N+:16]([O-:18])=[O:17])=[CH:4][CH:3]=1.[Cl:19]C(Cl)Cl>>[ClH:19].[F:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:8][NH:9][C:10]2[CH:11]=[N:12][CH:13]=[CH:14][C:15]=2[N+:16]([O-:18])=[O:17])=[CH:6][CH:7]=1

Komponenten

3

Edukt 2

HCID 6212Chloroform2×HCID 156147143-(4-Fluorobenzylamino)-4-nitropyridine

Produkt 1

HCID 15614715HCID 15614715, Verbindung

Versuchsvorschrift

To a stirred and cooled (0° C.) solution of 8.7 parts of N-[(4-fluorophenyl)methyl]-4-nitro-3-pyridinamine, 1-oxide and 150 parts of trichloromethane was added dropwise a solution of 10.2 parts of phosphor trichloride in 75 parts of trichloromethane. Upon completion, the mixture was allowed to reach room temperature and stirring was continued for one hour at reflux temperature. The reaction mixture was cooled and the solvent was evaporated. The residue was stirred in trichloromethane. The product was filtered off and dried, yielding 9 parts of N-[(4-fluorophenyl)methyl]-4-nitro-3-pyridinamine monohydrochloride (intermediate 13).

Aufarbeitung

  1. customto reach room temperature
  2. stirringstirring
  3. temperatureat reflux temperature
  4. temperatureThe reaction mixture was cooled
  5. customthe solvent was evaporated
  6. stirringThe residue was stirred in trichloromethane
  7. filtrationThe product was filtered off
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-60823f941e484dedb5cff085cb0583cd
Quelldatensatz
uspto-grants-1989_12
Patentnummer
US04888426

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