Reaktionsgleichung
[CH2:1]([NH:3][CH2:4][CH3:5])C.C1([N:12]=C=NC2CCCCC2)CCCCC1.[ClH:21].[NH2:22][CH:23]([C:46]([O:48][CH3:49])=[O:47])[CH2:24][C:25]1[CH:45]=[CH:44][C:28]([O:29][C:30]2[CH:43]=[CH:42][C:33]([CH:34]=[C:35]3[S:39][C:38](=[O:40])[NH:37][C:36]3=[O:41])=[CH:32][CH:31]=2)=[CH:27][CH:26]=1.[OH:50][C:51]1[C:59]2[N:58]=NN[C:55]=2C=CC=1>CN(C)C=O>[ClH:21].[ClH:21].[NH2:58][CH:59]([CH2:55][C:4]1[N:3]=[CH:1][NH:12][CH:5]=1)[C:51]([NH:22][CH:23]([C:46]([O:48][CH3:49])=[O:47])[CH2:24][C:25]1[CH:45]=[CH:44][C:28]([O:29][C:30]2[CH:43]=[CH:42][C:33]([CH2:34][CH:35]3[S:39][C:38](=[O:40])[NH:37][C:36]3=[O:41])=[CH:32][CH:31]=2)=[CH:27][CH:26]=1)=[O:50]Komponenten
6
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
Diethylamine (1.04 ml, 6.0 mmol) and N,N′-dicyclohexylcarbodiimide (0.64 g, 3.13 mmol) were added to the stirred suspension of 5-[4-(4-(2-amino-2-methoxycarbonylethyl)phenoxy)benzylidene]thiazolidin-2,4-dione hydrochloride (1.3 g, 3.0 mmol), 2-N-t-butoxycarbonylamino-4-imidazole propionic acid (0.8 g, 3.13 mmol) and hydroxylbenzotriazole (0.42 g, 3.13 mmol) in N,N-dimethyl formamide (15 ml). The stirring was continued for 24 h and the reaction mixture was concentrated in vacuum. The obtained residue was washed with 10% sodium bicarbonate, brine and purified with preparative HPLC to yield the title compound (1.5 g, yield 79%).
Aufarbeitung
- concentrationthe reaction mixture was concentrated in vacuum
- washThe obtained residue was washed with 10% sodium bicarbonate, brine
- custompurified with preparative HPLC
Quellen und Nachweise
- ORD-Eintrag
- ord-b7b3ed40ed644461b6f858f1a00c0109
- Quelldatensatz
- uspto-grants-2006_08
- Patentnummer
- US07087576B2
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