Piperidine → HCID 21490881, Verbindung

HRID 1973897Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1973897
[OH:1][CH2:2][C:3]1[CH:8]=[C:7]([Cl:9])[C:6]([CH2:10][CH2:11][CH2:12][CH3:13])=[C:5](Cl)[N:4]=1.[NH:15]1[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]1>>[OH:1][CH2:2][C:3]1[CH:8]=[C:7]([Cl:9])[C:6]([CH2:10][CH2:11][CH2:12][CH3:13])=[C:5]([N:15]2[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]2)[N:4]=1

Komponenten

3

Edukt 2

HCID 8082PiperidineHCID 21490887HCID 21490887, Verbindung

Produkt 1

HCID 21490881HCID 21490881, Verbindung

Versuchsvorschrift

46.8 g (0.2 mol) of 2-hydroxymethyl-4,6-dichloro-5-n-butyl-pyridine dissolved in 425 g (5 mols) of piperidine are heated for 20 hours at 190° in a bomb tube. The reaction mixture is then evaporated and the piperidine which still adheres is distilled off by means of toluene. The residue is rendered alkaline with 2 N sodium carbonate solution and the mixture is extracted with ether. The ether phases are combined, dried over sodium sulphate, filtered and evaporated. Fractional distillation of the residue in a high vacuum yields 2-hydroxymethyl-4-chloro-5-n-butyl-6-piperidino-pyridine of the formula ##STR17## and of boiling point 147°-152° (0.25 mm Hg).

Aufarbeitung

  1. temperatureare heated for 20 hours at 190° in a bomb tube
  2. customThe reaction mixture is then evaporated
  3. distillationthe piperidine which still adheres is distilled off by means of toluene
  4. extractionthe mixture is extracted with ether
  5. dry with materialdried over sodium sulphate
  6. filtrationfiltered
  7. customevaporated
  8. distillationFractional distillation of the residue in a high vacuum

Quellen und Nachweise

ORD-Eintrag
ord-8dec4c71afc64d7ba1dff8a8ffe43259
Quelldatensatz
uspto-grants-1976_12
Patentnummer
US03998955

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