Trifluoroacetic acid → HCID 68616622, Verbindung

HRID 1620060Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1620060
C(O)(C(F)(F)F)=O.C(OC(=O)[NH:14][C:15]1[CH:16]=[N:17][CH:18]=[C:19]([C:21]2[O:22][C:23]([CH3:26])=[CH:24][CH:25]=2)[CH:20]=1)(C)(C)C>C(Cl)(Cl)Cl>[CH3:26][C:23]1[O:22][C:21]([C:19]2[CH:20]=[C:15]([NH2:14])[CH:16]=[N:17][CH:18]=2)=[CH:25][CH:24]=1

Komponenten

4

Edukt 2

HCID 6422Trifluoroacetic acidHCID 89546857HCID 89546857, Verbindung

Produkt 1

HCID 68616622HCID 68616622, VerbindungAusbeute 118,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Versuchsvorschrift

TFA (1 ml) was added to a chloroform solution (2 ml) containing tert-butyl(5-(5-methylfuran-2-yl)pyridin-3-yl)carbamate (61 mg) obtained in the 1st step, stirring at room temperature for 2 hours. The solvent was distilled away under reduced pressure, the obtained residue was dissolved in chloroform, and the resultant was washed with water and a saturated aqueous sodium hydrogen carbonate solution. Subsequently, the aqueous layers were combined, followed by extraction with chloroform (×2). The organic layers was combined and dried over anhydrous sodium sulfate. The solvent was distilled away from the obtained organic layers under reduced pressure, and a white solid of 5-(5-methylfuran-2-yl)pyridin-3-amine (46 mg) was thus obtained.

Aufarbeitung

  1. customobtained in the 1st step
  2. distillationThe solvent was distilled away under reduced pressure
  3. dissolutionthe obtained residue was dissolved in chloroform
  4. washthe resultant was washed with water
  5. extractionfollowed by extraction with chloroform (×2)
  6. dry with materialdried over anhydrous sodium sulfate
  7. distillationThe solvent was distilled away from the obtained organic layers under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-c57bd9764d5340459d7bed388b3cc92d
Quelldatensatz
uspto-grants-2014_07
Patentnummer
US08772320B2

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