Tetrabutylammonium permanganate → HCID 19072548, Verbindung

HRID 1955741Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1955741
[C:1]1([CH3:38])[CH:6]=[CH:5][C:4]([S:7]([NH:10][C:11](=[O:37])[CH:12]([C:18]2[CH:23]=[CH:22][C:21]([CH2:24][N:25]3[C:29]([CH:30]=[O:31])=[C:28]([Cl:32])[N:27]=[C:26]3[CH2:33][CH2:34][CH2:35][CH3:36])=[CH:20][CH:19]=2)[CH:13]2[CH2:17][CH2:16][CH2:15][CH2:14]2)(=[O:9])=[O:8])=[CH:3][CH:2]=1.[Mn]([O-])(=O)(=O)=[O:40].C([N+](CCCC)(CCCC)CCCC)CCC>N1C=CC=CC=1>[C:1]1([CH3:38])[CH:2]=[CH:3][C:4]([S:7]([NH:10][C:11](=[O:37])[CH:12]([C:18]2[CH:23]=[CH:22][C:21]([CH2:24][N:25]3[C:29]([C:30]([OH:40])=[O:31])=[C:28]([Cl:32])[N:27]=[C:26]3[CH2:33][CH2:34][CH2:35][CH3:36])=[CH:20][CH:19]=2)[CH:13]2[CH2:17][CH2:16][CH2:15][CH2:14]2)(=[O:9])=[O:8])=[CH:5][CH:6]=1

Komponenten

4

Edukt 2

HCID 11760202Tetrabutylammonium permanganateHCID 19072485N-4-Tolylsulphonyl-2-[4-(2-butyl-4-chloro-5-formyl-imidazol-1-yl-methyl)-phenyl]-2-cyclopentyl-acetamide

Produkt 1

HCID 19072548HCID 19072548, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel2×

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

250 mg (0.45 mmol) of the compound from Example III are dissolved in 2.5 ml (0.45 mmol) of pyridine and 162 mg of tetrabutylammonium permanganate, dissolved in 1.5 ml of pyridine, are added at 60° C., and the mixture is stirred at 60° C. for 2 h. The pyridine is evaporated, and the residue is taken up in water, acidified with dilute HCl and extracted with ethyl acetate. The organic phase is concentrated and the residue is chromatographed on silica gel 60 using CH2Cl2 /MeOH (10:1).

Aufarbeitung

  1. additionare added at 60° C.
  2. customThe pyridine is evaporated
  3. extractionextracted with ethyl acetate
  4. concentrationThe organic phase is concentrated
  5. customthe residue is chromatographed on silica gel 60 using CH2Cl2 /MeOH (10:1)

Quellen und Nachweise

ORD-Eintrag
ord-f55a8a9747e94994b369373934dccc4c
Quelldatensatz
uspto-grants-1998_07
Patentnummer
US05776964

Notizen zur Reaktion

Wird geladen…