Hydrochloric Acid → HCID 22009947, Verbindung

HRID 322091Notizen

Reaktionsgleichung

[OH-].[Na+].[O:3]1[C:7]2[CH:8]=[CH:9][C:10]([CH:12]([C:28]3[C:36]4[C:31](=[CH:32][C:33]([C:37]([O:39]C)=[O:38])=[CH:34][CH:35]=4)[N:30]([CH3:41])[CH:29]=3)[C:13]([NH:15][S:16]([C:19]3[CH:24]=[CH:23][C:22]([CH3:25])=[CH:21][C:20]=3[O:26][CH3:27])(=[O:18])=[O:17])=[O:14])=[CH:11][C:6]=2[O:5][CH2:4]1.Cl>CO.O.ClCCl>[O:3]1[C:7]2[CH:8]=[CH:9][C:10]([CH:12]([C:28]3[C:36]4[C:31](=[CH:32][C:33]([C:37]([OH:39])=[O:38])=[CH:34][CH:35]=4)[N:30]([CH3:41])[CH:29]=3)[C:13]([NH:15][S:16]([C:19]3[CH:24]=[CH:23][C:22]([CH3:25])=[CH:21][C:20]=3[O:26][CH3:27])(=[O:17])=[O:18])=[O:14])=[CH:11][C:6]=2[O:5][CH2:4]1

Komponenten

Reaktionsbedingungen

Temperatur: 45 °C

Versuchsvorschrift

Aqueous sodium hydroxide (9.0 liters of a 20% aqueous solution) was added to a stirred suspension of methyl 3-{1-(1,3-benzodioxol-5-yl)-2-[(2-methoxy4-methylphenyl)-sulfonylamino]-2-oxoethyl}-1-methyl-1H-indole-6-carboxylate (from step (b), 5.0 kg) in methanol (25 liters) and demineralised water (20 liters). The suspension was warmed to 45° C. for 1.5 h, cooled to room temperature and diluted with dichloromethane (25 liters). The pH of the aqueous phase was adjusted to 3 with the addition of concentrated hydrochloric acid (7.0 liters) and the phases separated. The organic phase was concentrated to low volume and filtration of the precipitated product gave the subtitle compound as a white crystalline solid (4.5 kg, 92%).

Aufarbeitung

temperaturecooled to room temperature
customthe phases separated
concentrationThe organic phase was concentrated to low volume and filtration of the precipitated product

Quellen und Nachweise

ORD-Eintrag: ord-28c678a1082440e2872b6f2bf976e2a3
Quelldatensatz: uspto-grants-2001_04
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US06211223B1

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