Hydrogen chloride-ethyl acetate → HCID 67398869, Verbindung

HRID 1426827Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1426827
[F:1][C:2]1[C:3]([CH2:23][N:24](C)[C:25](=O)OC(C)(C)C)=[CH:4][N:5]([S:14]([C:17]2[CH:21]=[CH:20][O:19][C:18]=2[CH3:22])(=[O:16])=[O:15])[C:6]=1[C:7]1[C:8]([F:13])=[N:9][CH:10]=[CH:11][CH:12]=1.C(OCC)(=O)C.[ClH:39]>C(OCC)(=O)C.C(O)C>[ClH:39].[F:1][C:2]1[C:3]([CH2:23][NH:24][CH3:25])=[CH:4][N:5]([S:14]([C:17]2[CH:21]=[CH:20][O:19][C:18]=2[CH3:22])(=[O:16])=[O:15])[C:6]=1[C:7]1[C:8]([F:13])=[N:9][CH:10]=[CH:11][CH:12]=1

Komponenten

5

Edukt 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 67397409HCID 67397409, Verbindung

Produkt 1

HCID 67398869HCID 67398869, VerbindungAusbeute 78 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

tert-Butyl ({4-fluoro-5-(2-fluoropyridin-3-yl)-1-[(2-methyl-3-furyl)sulfonyl]-1H-pyrrol-3-yl}methyl)methylcarbamate (187 mg) was dissolved in ethyl acetate (1 mL) and ethanol (1 mL), and 4 mol/L hydrogen chloride-ethyl acetate solution (2 mL) was added. The mixture was stirred at room temperature for 2 hr, and the reaction mixture was concentrated under reduced pressure. The residue was recrystallized from a mixed solvent of ethyl acetate-ethanol=3:1 to give the title compound as colorless crystals (yield 125 mg, 78%).

Aufarbeitung

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. customThe residue was recrystallized from a mixed solvent of ethyl acetate-ethanol=3:1

Quellen und Nachweise

ORD-Eintrag
ord-c460bef8f2944d259f176633c1b59773
Quelldatensatz
uspto-grants-2015_01
Patentnummer
US08933105B2

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