Citric Acid → HCID 59135672, Verbindung

HRID 1960317

Reaktionsgleichung

C([O:3][C:4](=[O:36])[CH2:5][N:6]1[CH2:11][CH2:10][N:9]([CH2:12][C:13]2[S:17][C:16]([C:18]3[NH:19][C:20]4[C:25]([CH:26]=3)=[CH:24][CH:23]=[CH:22][C:21]=4[NH:27][S:28]([C:31]3[S:32][CH:33]=[CH:34][CH:35]=3)(=[O:30])=[O:29])=[N:15][CH:14]=2)[CH2:8][CH2:7]1)C.[OH-].[Na+].C(O)(=O)CC(CC(O)=O)(C(O)=O)O.[Cl-].[Na+]>O1CCCC1.C(OCC)(=O)C.CO>[S:32]1[CH:33]=[CH:34][CH:35]=[C:31]1[S:28]([NH:27][C:21]1[CH:22]=[CH:23][CH:24]=[C:25]2[C:20]=1[NH:19][C:18]([C:16]1[S:17][C:13]([CH2:12][N:9]3[CH2:10][CH2:11][N:6]([CH2:5][C:4]([OH:36])=[O:3])[CH2:7][CH2:8]3)=[CH:14][N:15]=1)=[CH:26]2)(=[O:29])=[O:30]

Komponenten

Reaktionsbedingungen

Temperatur: 50 °C

Versuchsvorschrift

To a solution of ethyl{4-[(2-{7-[(2-thienylsulfonyl)amino]-1H-indol-2-yl}-1,3-thiazol-5-yl)methyl]piperazin-1-yl}acetate (0.500 g) in a mixed solvent of tetrahydrofuran (15 ml) and methanol (5 ml) was added 2N aqueous sodium hydroxide solution (1.5 ml), and the mixture was stirred at 50° C. for 2 hr. 10% Aqueous citric acid solution, ethyl acetate, sodium chloride and tetrahydrofuran were successively added to the reaction solution, and the precipitated crystals were collected by filtration, washed with ethyl acetate, and dried to give the title compound (0.360 g, yield 76%) as colorless crystals.

Aufarbeitung

filtrationthe precipitated crystals were collected by filtration
washwashed with ethyl acetate
customdried

Quellen und Nachweise

ORD-Eintrag: ord-be3bb0865fd24c32b5488e8599f76ffd
Quelldatensatz: uspto-grants-2013_04
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US08410087B2

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