Diethyl (2-cyanoethyl)(3,4-difluorophenyl)propanedioate → Ethyl 3-(3,4-difluorophenyl)-2-oxopiperidine-3-carboxylate

HRID 71110

Reaktionsgleichung

Reaktionsgleichung von HRID 71110
[C:1]([CH2:3][CH2:4][C:5]([C:16]1[CH:21]=[CH:20][C:19]([F:22])=[C:18]([F:23])[CH:17]=1)([C:11]([O:13][CH2:14][CH3:15])=[O:12])[C:6](OCC)=[O:7])#[N:2]>[Co].N>[F:23][C:18]1[CH:17]=[C:16]([C:5]2([C:11]([O:13][CH2:14][CH3:15])=[O:12])[CH2:4][CH2:3][CH2:1][NH:2][C:6]2=[O:7])[CH:21]=[CH:20][C:19]=1[F:22]

Komponenten

4

Edukt 1

HCID 66608241Diethyl (2-cyanoethyl)(3,4-difluorophenyl)propanedioate

Produkt 1

HCID 66607999Ethyl 3-(3,4-difluorophenyl)-2-oxopiperidine-3-carboxylateAusbeute 79,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 104730CobaltKatalysatorHCID 222AmmoniaLösungsmittel

Versuchsvorschrift

A mixture of diethyl (2-cyanoethyl)(3,4-difluorophenyl)propanedioate (15.2 g), Raney cobalt (75 g) and ammonia (2M ethanol solution, 150 mL) was stirred at room temperature for 3 days under a hydrogen atmosphere. The insoluble material was filtered off through celite, and the filtrate was concentrated under reduced pressure. The residue was washed with diisopropylether to give the title compound (10.5 g).

Aufarbeitung

  1. filtrationThe insoluble material was filtered off through celite
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. washThe residue was washed with diisopropylether

Quellen und Nachweise

ORD-Eintrag
ord-42390afab45e45948b53e8b96a946d2e
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08822699B2

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