Ammonia → 5-(3,4-Dichlorobutyl)pyridine-2-carboxamide

HRID 1580974Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1580974
[Cl:1][CH:2]([CH2:14][Cl:15])[CH2:3][CH2:4][C:5]1[CH:6]=[CH:7][C:8]([C:11](O)=[O:12])=[N:9][CH:10]=1.S(Cl)(Cl)=O.C(Cl)(Cl)Cl.[NH3:24]>C1C=CC=CC=1>[Cl:1][CH:2]([CH2:14][Cl:15])[CH2:3][CH2:4][C:5]1[CH:6]=[CH:7][C:8]([C:11]([NH2:24])=[O:12])=[N:9][CH:10]=1

Komponenten

6

Edukt 4

HCID 222AmmoniaHCID 6212ChloroformHCID 24386Thionyl ChlorideHCID 2181975-(3,4-Dichlorobutyl)pyridine-2-carboxylic acid

Produkt 1

HCID 132718785-(3,4-Dichlorobutyl)pyridine-2-carboxamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 241BenzeneLösungsmittel

Versuchsvorschrift

10 g of 5-(3,4-dichlorobutyl)picolinic acid was added to the solution of thionyl chloride (30 ml) and chloroform (100 ml), and resulting solution was refluxed for fifteen minutes. The reaction mixture was evaporated in reduced pressure to obtain oily residue. This was dissolved in 100 ml of benzene and treated with 28% aqueous ammonia (50 ml) at 4° - 10°C with vigorous stirring for an hour. Benzene extract was evaporated in reduced pressure to give crude product as solid.

Aufarbeitung

  1. customresulting solution
  2. temperaturewas refluxed for fifteen minutes
  3. customThe reaction mixture was evaporated in reduced pressure
  4. customto obtain oily residue
  5. extractionBenzene extract
  6. customwas evaporated in reduced pressure
  7. customto give crude product as solid

Quellen und Nachweise

ORD-Eintrag
ord-199681186ad64a948c28d562c5d279a8
Quelldatensatz
uspto-grants-1976_01
Patentnummer
US03935221

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