Trifluoroacetic acid → HCID 178511513, Verbindung

HRID 72849

Reaktionsgleichung

Reaktionsgleichung von HRID 72849
C(OC(=O)[NH:7][C@H:8]1[CH2:13][CH2:12][C@H:11]([CH2:14][CH2:15][N:16]2[CH2:21][CH2:20][CH:19]([C:22]3[C:26]4[CH:27]=[C:28]([F:31])[CH:29]=[CH:30][C:25]=4[O:24][N:23]=3)[CH2:18][CH2:17]2)[CH2:10][CH2:9]1)(C)(C)C.[F:33][C:34]([F:39])([F:38])[C:35]([OH:37])=[O:36].C([O-])(O)=O.[Na+]>ClCCl>[F:33][C:34]([F:39])([F:38])[C:35]([OH:37])=[O:36].[F:31][C:28]1[CH:29]=[CH:30][C:25]2[O:24][N:23]=[C:22]([CH:19]3[CH2:20][CH2:21][N:16]([CH2:15][CH2:14][C@H:11]4[CH2:12][CH2:13][C@H:8]([NH2:7])[CH2:9][CH2:10]4)[CH2:17][CH2:18]3)[C:26]=2[CH:27]=1

Komponenten

5

Edukt 3

HCID 6422Trifluoroacetic acidHCID 516892Sodium BicarbonateHCID 178453892HCID 178453892, Verbindung

Produkt 1

HCID 178511513HCID 178511513, VerbindungAusbeute 100 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

2.3 g (5 mmol) of trans(4-{2-[4-(5-Fluoro-benzo[d]isoxazol-3-yl)-piperidin-1-yl]-ethyl}-cyclohexyl)-carbamic acid tert-butyl ester is solved in dichloromethane (15 mL) and trifluoroacetic acid is added at 0° C. (10.7 mL, 46 mmol) and the mixture is stirred at room temperature overnight. NaHCO3 is slowly added until pH 9 and the mixture extracted 3 times with dichloromethane and ethyl acetate. The solvent was evaporated to yield 1.86 g (5.3 mmol, 100%) of a white solid that was used without purification on the next steps. MS (m/e): 346.3 (M+H+).

Aufarbeitung

  1. extractionthe mixture extracted 3 times with dichloromethane and ethyl acetate
  2. customThe solvent was evaporated

Quellen und Nachweise

ORD-Eintrag
ord-f164707f5cf149de9a220c8349c714a3
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08829029B2

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