Hydroxide → HCID 59007054, Verbindung

HRID 130477Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 130477
[CH3:1][C@H:2]1[NH:7][C@@H:6]([CH3:8])[CH2:5][N:4]([C:9]2[CH:10]=[CH:11][C:12]([O:31]CC3C=CC=CC=3)=[C:13]([NH:15][S:16]([C:19]3[CH:24]=[CH:23][C:22]([C:25]4[O:26][C:27]([CH3:30])=[CH:28][CH:29]=4)=[CH:21][CH:20]=3)(=[O:18])=[O:17])[CH:14]=2)[CH2:3]1.[OH-]>C(O)C.CN(C)C=O>[CH3:8][C@H:6]1[NH:7][C@@H:2]([CH3:1])[CH2:3][N:4]([C:9]2[CH:10]=[CH:11][C:12]([OH:31])=[C:13]([NH:15][S:16]([C:19]3[CH:24]=[CH:23][C:22]([C:25]4[O:26][C:27]([CH3:30])=[CH:28][CH:29]=4)=[CH:21][CH:20]=3)(=[O:18])=[O:17])[CH:14]=2)[CH2:5]1

Komponenten

5

Edukt 2

HCID 961HydroxideHCID 69196742HCID 69196742, Verbindung

Produkt 1

HCID 59007054HCID 59007054, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A solution of N-{5-(cis-3,5-dimethyl-1-piperazinyl)-2-[(phenylmethyl)oxy]phenyl}-4-(5-methyl-2-furanyl)benzenesulfonamide (D43) (100 mg, 0.19 mmol) in ethanol (4 ml) and N,N-dimethylformamide (2.5 ml) was treated with palladiwn hydroxide on carbon (25 mg) and the mixture stirred under an atmosphere of hydrogen for 3.75 h. The mixture was then filtered through celite, washing with ethanol and the filtrate reduced in vacuo and the residue purified by mass directed autoprep HPLC to afford the title compound. MS (ES+) m/e 442 [M+H]+.

Aufarbeitung

  1. filtrationThe mixture was then filtered through celite
  2. washwashing with ethanol
  3. customthe residue purified by mass

Quellen und Nachweise

ORD-Eintrag
ord-a8519bb8b1e6467eaa8551e0b0d993c5
Quelldatensatz
uspto-grants-2008_06
Patentnummer
US07381728B2

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