Trifluoroacetic acid → HCID 21100737, Verbindung

HRID 1352513Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1352513
FC(F)(F)C(O)=O.C(OC(=O)[NH:14][C:15]1[CH:20]=[CH:19][C:18]([C:21]2[C:25]([CH2:26][C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)=[CH:24][O:23][N:22]=2)=[CH:17][CH:16]=1)(C)(C)C>>[CH2:26]([C:25]1[C:21]([C:18]2[CH:17]=[CH:16][C:15]([NH2:14])=[CH:20][CH:19]=2)=[N:22][O:23][CH:24]=1)[C:27]1[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=1

Komponenten

3

Versuchsvorschrift

Trifluoroacetic acid (0.5 mL) is added to [4-(4-benzylisoxazol-3-yl)phenyl]carbamic acid tert-butyl ester (0.3 g) and stirred for 30 minutes. The reaction mixture is concentrated under reduced pressure and the concentrate is partitioned between ethyl acetate and 1N sodium hydroxide solution. The organic layer is washed with saturated sodium chloride, dried over anhydrous magnesium sulfate and chromatographed on silica gel (ethyl acetate/hexane as eluant) to give 0.15 g product as a white solid. MS: m/z 251 (M+H)+.

Aufarbeitung

  1. concentrationThe reaction mixture is concentrated under reduced pressure
  2. customthe concentrate is partitioned between ethyl acetate and 1N sodium hydroxide solution
  3. washThe organic layer is washed with saturated sodium chloride
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customchromatographed on silica gel (ethyl acetate/hexane as eluant)

Quellen und Nachweise

ORD-Eintrag
ord-c517227dcce74e24ba87c98372128d96
Quelldatensatz
uspto-grants-2007_05
Patentnummer
US07220768B2

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