Piperidine → HCID 67187268, Verbindung

HRID 451616Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 451616
F[C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[F:11])[C:7](=[O:12])[CH2:6][CH2:5]2.[NH:13]1[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]1>N1C=CC=CC=1>[F:11][C:10]1[CH:9]=[C:8]2[C:4]([CH2:5][CH2:6][C:7]2=[O:12])=[CH:3][C:2]=1[N:13]1[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]1

Komponenten

4

Edukt 2

HCID 8082PiperidineHCID 117689445,6-Difluoro-1-indanone

Produkt 1

HCID 67187268HCID 67187268, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

5,6-difluoro-indan-1-one (2.49 g, 14.8 mmol) and piperidine (4.4 ml, 3.78 g, 44.4 mmol) were dissolved in pyridine (10 ml) and heated to reflux for 16 hours. The reaction was cooled, and the solvent removed under vacuum. The residue was taken in ethyl ether, washed with 1N aqueous sodium hydroxide and water, dried with magnesium sulfate, and the solvent removed under vacuum to give the desired product as 2.97 g of a black solid that was used without further purification. 1H NMR (300 MHz, CDCl3) 7.32 (d, 1H), 6.88 (d, 1H), 3.19 (m, 4H), 3.03 (m, 2H), 2.66 (m, 2H), 1.73 (m, 4H), 1.62 (m, 2H). MS (CSI) m/e 234 (M+H)+

Aufarbeitung

  1. temperatureheated
  2. temperatureto reflux for 16 hours
  3. temperatureThe reaction was cooled
  4. customthe solvent removed under vacuum
  5. washwashed with 1N aqueous sodium hydroxide and water
  6. dry with materialdried with magnesium sulfate
  7. customthe solvent removed under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-b394b8a175d84154a5a9758629da0424
Quelldatensatz
uspto-grants-2013_07
Patentnummer
US08487116B2

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