HCID 86583958, Verbindung → 2,2,2-Trifluoro-1-[4-(6-methoxy-3,4-dihydro-isoquinolin-1-yl)-piperidin-1-yl]-ethanone

HRID 397061

Reaktionsgleichung

Reaktionsgleichung von HRID 397061
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:9][CH2:10][NH:11][C:12]([CH:14]2[CH2:19][CH2:18][N:17]([C:20](=[O:25])[C:21]([F:24])([F:23])[F:22])[CH2:16][CH2:15]2)=O)[CH:6]=[CH:7][CH:8]=1>O=P(Cl)(Cl)Cl>[F:22][C:21]([F:24])([F:23])[C:20]([N:17]1[CH2:18][CH2:19][CH:14]([C:12]2[C:6]3[C:5](=[CH:4][C:3]([O:2][CH3:1])=[CH:8][CH:7]=3)[CH2:9][CH2:10][N:11]=2)[CH2:15][CH2:16]1)=[O:25]

Komponenten

3

Edukt 1

HCID 86583958HCID 86583958, Verbindung

Produkt 1

HCID 181723932,2,2-Trifluoro-1-[4-(6-methoxy-3,4-dihydro-isoquinolin-1-yl)-piperidin-1-yl]-ethanoneAusbeute 88,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 24813Phosphorus oxychlorideLösungsmittel

Versuchsvorschrift

A stirred solution of 1-trifluoroacetyl-piperidine-4-carboxylic acid [2-(3-methoxy-phenyl)-ethyl]-amide (1.04 g, 2.9 mmol) in POCl3 under an atmosphere of N2 was heated at reflux for 2.5 hours. The reaction was allowed to cool to RT and the POCl3 was removed in vacuo. The residual oil was suspended in toluene (20 ml) and concentrated in vacuo (this process was repeated twice more), leaving the desired product as a tan colored solid (0.872 g, 2.56 mmol, 88% yield). MS 341 (M+1)

Aufarbeitung

  1. temperatureat reflux for 2.5 hours
  2. customthe POCl3 was removed in vacuo
  3. concentrationconcentrated in vacuo (this process

Quellen und Nachweise

ORD-Eintrag
ord-e2ab688b7a3f4015909250ff6dcb8c4d
Quelldatensatz
uspto-grants-2003_08
Patentnummer
US06608203B2

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