Phosphorus oxychloride → HCID 178506089, Verbindung

HRID 496256

Reaktionsgleichung

Reaktionsgleichung von HRID 496256
[F:1][C:2]([F:14])([F:13])[C:3]1[CH:12]=[CH:11][C:6]2[NH:7][C:8](=O)[NH:9][C:5]=2[CH:4]=1.O=P(Cl)(Cl)[Cl:17]>>[Cl:17][C:8]1[NH:7][C:6]2[CH:11]=[CH:12][C:3]([C:2]([F:14])([F:13])[F:1])=[CH:4][C:5]=2[N:9]=1

Komponenten

3

Edukt 2

HCID 24813Phosphorus oxychlorideHCID 118201505-Trifluoromethyl-1,3-dihydro-benzimidazol-2-one

Produkt 1

HCID 178506089HCID 178506089, Verbindung

Versuchsvorschrift

Reflux 5-trifluoromethyl-1,3-dihydro-benzimidazol-2-one (17 g; Meanwell et al. (1995) J. Org. Chem. 60(6):1565-1582) for 14 hours in POCl3 (200 mL). Evaporate the solvent in vacuo, then carefully neutralize with saturated NaHCO3, and extract with EtOAc. Dry over Na2SO4, concentrate under vacuum, and purify by flash chromatography (1:1 hexanes/EtOAc) to obtain 2-chloro-5-trifluoromethyl-1H-benzimidazole. B. 1′-(5-Trifluoromethyl-1H-benzimidazol-2-yl)-spiro[isobenzofuran-1,4′-piperidin]-3-one hydrochloride

Aufarbeitung

  1. customEvaporate the solvent in vacuo
  2. extractionextract with EtOAc
  3. dry with materialDry over Na2SO4
  4. concentrationconcentrate under vacuum
  5. custompurify by flash chromatography (1:1 hexanes/EtOAc)

Quellen und Nachweise

ORD-Eintrag
ord-71967602e6af4430b1cc7bd91ac17548
Quelldatensatz
uspto-grants-2005_09
Patentnummer
US06943199B2

Verknüpfte Notizen

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