Potassium Carbonate → HCID 57935976, Verbindung

HRID 1434593Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1434593
Cl[CH2:2][CH2:3][C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=[O:5].[CH3:12][S:13]([C:16]1[CH:30]=[CH:29][C:19]2[N:20]([CH:23]3[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]3)[CH:21]=[N:22][C:18]=2[CH:17]=1)(=[O:15])=[O:14].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH3:12][S:13]([C:16]1[CH:30]=[CH:29][C:19]2[N:20]([CH:23]3[CH2:24][CH2:25][N:26]([CH2:2][CH2:3][C:4]([C:6]4[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=4)=[O:5])[CH2:27][CH2:28]3)[CH:21]=[N:22][C:18]=2[CH:17]=1)(=[O:15])=[O:14]

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 702953-ChloropropiophenoneHCID 58998518HCID 58998518, Verbindung

Produkt 1

HCID 57935976HCID 57935976, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

3-Chloropropiophenone (860 mg) was added to a mixture of 5-(methylsulfonyl)-1-piperidin-4-yl-1H-benzimidazole (1.395 g) and potassium carbonate (1.38 g) in DMF (30 ml) and stirred for 2 days. The reaction mixture was evaporated to dryness and the residue was dissolved in dichloromethane (20 ml), washed with water (15 ml) and brine (15 ml), dried and evaporated to dryness to give the title compound, yield 2.07 g, M+H 412, NMR (CDCl3) 2.2 (m, 4H) 2.3-2.4 (m, 2H) 2.9 (m, 2H) 3.1 (s, 3H) 3.2-3.3 (m, 4H) 4.3 (m, 1H) 7.5 (m, 2H) 7.6 (m, 2H) 7.9 (m, 2H) 8.0 (m, 1H) 8.2 (s, 1H) 8.4 (s, 1H).

Aufarbeitung

  1. customThe reaction mixture was evaporated to dryness
  2. dissolutionthe residue was dissolved in dichloromethane (20 ml)
  3. washwashed with water (15 ml) and brine (15 ml)
  4. customdried
  5. customevaporated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-7fb6528ba5244589b175c6f75cd62349
Quelldatensatz
uspto-grants-2009_11
Patentnummer
US07615555B2

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