1-Butanaminium, N,N,N-tributyl-, fluoride, hydrate → HCID 16222146, Verbindung

HRID 1717392Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1717392
Br[CH2:2][CH2:3][CH2:4][C:5]1[N:9]([C:10]2[CH:15]=[CH:14][C:13]([C:16]([NH:18][CH2:19][C:20]([F:23])([F:22])[F:21])=[O:17])=[CH:12][CH:11]=2)[N:8]=[N:7][C:6]=1[C:24]([NH:26][CH:27]1[CH2:29][CH2:28]1)=[O:25].O.[F-].C([N+](CCCC)(CCCC)CCCC)CCC>C(#N)C>[CH:27]1([NH:26][C:24]([C:6]2[N:7]=[N:8][N:9]([C:10]3[CH:15]=[CH:14][C:13]([C:16]([NH:18][CH2:19][C:20]([F:21])([F:22])[F:23])=[O:17])=[CH:12][CH:11]=3)[C:5]=2/[CH:4]=[CH:3]/[CH3:2])=[O:25])[CH2:29][CH2:28]1

Komponenten

4

Edukt 2

HCID 162116731-Butanaminium, N,N,N-tributyl-, fluoride, hydrateHCID 68514522HCID 68514522, Verbindung

Produkt 1

HCID 16222146HCID 16222146, VerbindungAusbeute 16 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

5-(3-Bromopropyl)-N-cyclopropyl-1-(4-{[(2,2,2-trifluoroethyl)amino]carbonyl}phenyl)-1H-1,2,3-triazole-4-carboxamide (212 mg, 0.45 mmol) obtained in Example 399a) was dissolved in acetonitrile (5.0 ml), tetrabutylammonium fluoride monohydrate (140 mg, 0.54 mmol) was added, and the mixture was stirred at 80° C. for 16 hr. The reaction mixture was allowed to cool to room temperature and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column (ethyl acetate/hexane=1/9 to 7/3) and recrystallized from ethyl acetate-hexane to give the title compound as a colorless powder (27.7 mg, 16%).

Aufarbeitung

  1. temperatureto cool to room temperature
  2. customthe solvent was evaporated under reduced pressure
  3. customThe residue was purified by silica gel column (ethyl acetate/hexane=1/9 to 7/3)
  4. customrecrystallized from ethyl acetate-hexane

Quellen und Nachweise

ORD-Eintrag
ord-f3d877944089492ebc35e1a1f5528a93
Quelldatensatz
uspto-grants-2010_09
Patentnummer
US07803822B2

Notizen zur Reaktion

Wird geladen…