Phenyl chloroformate → HCID 13825039, Verbindung

HRID 648502Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 648502
[C:1](Cl)(=[O:9])[O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[Cl:11][CH:12]1[CH2:17][CH2:16][N:15](C)[CH2:14][CH2:13]1>C(Cl)Cl>[Cl:11][CH:12]1[CH2:17][CH2:16][N:15]([C:1]([O:2][C:3]2[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=2)=[O:9])[CH2:14][CH2:13]1

Komponenten

4

Edukt 2

HCID 15891Phenyl chloroformateHCID 793424-chloro-N-methylpiperidine

Produkt 1

HCID 13825039HCID 13825039, VerbindungAusbeute 71,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

A solution of phenyl chlorocarbonate (17.3 g) in dry methylene chloride (40 ml) was dropwise added to a stirred solution of 4-chloro-1-methylpiperidine (13.3 g) in dry methylene chloride (60 ml) under ice-cooling over a period of 5 minutes. The resultant mixture was stirred at the same temperature for 30 minutes and then at room temperature for 6 hours. The mixture was washed with water, dried over magnesium sulfate, and concentrated in vacuo to give an oil, which was distilled to give phenyl 4-chloro-1-piperidine-carboxylate (17.0 g) as a colourless oil.

Aufarbeitung

  1. temperaturecooling over a period of 5 minutes
  2. washThe mixture was washed with water
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. customto give an oil, which
  6. distillationwas distilled

Quellen und Nachweise

ORD-Eintrag
ord-6a1cf50a9ac142f78cea1743e926d14b
Quelldatensatz
uspto-grants-1988_04
Patentnummer
US04735952

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