Pyridine → HCID 23339068, Verbindung

HRID 26741Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 26741
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[NH:9][CH:10]1[CH2:15][CH2:14][N:13]([C:16]([O:18][CH2:19][CH3:20])=[O:17])[CH2:12][CH2:11]1.N1C=CC=CC=1.[C:27]1([CH2:33][C:34](Cl)=[O:35])[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1>C1C=CC=CC=1>[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[N:9]([CH:10]1[CH2:15][CH2:14][N:13]([C:16]([O:18][CH2:19][CH3:20])=[O:17])[CH2:12][CH2:11]1)[C:34](=[O:35])[CH2:33][C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1

Komponenten

5

Edukt 3

HCID 1049PyridineHCID 7679Phenylacetyl chlorideHCID 23338990HCID 23338990, Verbindung

Produkt 1

HCID 23339068HCID 23339068, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 241BenzeneLösungsmittel2×

Versuchsvorschrift

to a stirred solution of 8 parts of ethyl 4-[(2,6-dimethylphenyl)amino]-1-piperidinecarboxylate in 4 parts of pyridine and 80 parts of benzene are added dropwise 7.7 parts of benzeneacetyl chloride in 40 parts of benzene. After the addition is complete, the whole is heated to reflux and stirred at reflux temperature for 3h. 45. The reaction mixture is cooled and filtered. The benzene-phase is washed with water and then with sodium hydrogen carbonate solution and with water. After evaporation, an oily residue is obtained, which solidifies on triturating in 1,1'-oxybisethane, to yield 5 parts of ethyl 4-[N-(2,6-dimethylphenyl)-N-(phenylacetyl)amino]-1-piperidinecarboxylate; mp. 106° C.

Aufarbeitung

  1. additionAfter the addition
  2. temperaturethe whole is heated
  3. temperatureto reflux
  4. temperatureat reflux temperature for 3h
  5. temperatureThe reaction mixture is cooled
  6. filtrationfiltered
  7. washThe benzene-phase is washed with water
  8. customAfter evaporation
  9. customan oily residue is obtained
  10. customon triturating in 1,1'-oxybisethane

Quellen und Nachweise

ORD-Eintrag
ord-37c6f292c96845a9b52d30991246307e
Quelldatensatz
uspto-grants-1979_04
Patentnummer
US04151286

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