Reaktionsgleichung
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][CH2:9][C:10]([OH:12])=O)=[CH:4][CH:3]=1.[NH2:13][C@H:14]([C:19]([NH:21][CH2:22][C:23](O)=O)=[O:20])[CH2:15][CH:16]([CH3:18])[CH3:17].Cl.C1C=CC2N(O)N=[N:33]C=2C=1>CN(C)C=O.C(N(CC)CC)C>[C:23]([CH2:22][NH:21][C:19](=[O:20])[CH:14]([NH:13][C:10](=[O:12])[CH2:9][NH:8][C:5]1[CH:4]=[CH:3][C:2]([Cl:1])=[CH:7][CH:6]=1)[CH2:15][CH:16]([CH3:18])[CH3:17])#[N:33]Komponenten
7
Versuchsvorschrift
(4-Chloro-phenylamino)-acetic acid (0.5 g) and H-Leu-Gly((CN).HCl (0.55 g) are dissolved in dimethylformamide (4 ml). HOBt (0.44 g), WSCD.HCI (0.54 g), triethylamine (0.37 ml) is added and the reaction mixture is stirred for 18 hours. After evaporation of the solvent, the residue is extracted with ethyl acetate. The extract is washed with 10% citric acid, brine, sodium bicarbonate, brine and dried over magnesium sulfate and evaporated. The crude product is slurried in diethylether and the solid filtered of and dried (vacuum) yielding a white powder with mp. 131-134° C.
Aufarbeitung
- customAfter evaporation of the solvent
- extractionthe residue is extracted with ethyl acetate
- washThe extract is washed with 10% citric acid, brine, sodium bicarbonate, brine
- dry with materialdried over magnesium sulfate
- customevaporated
- filtrationthe solid filtered of and
- customdried (vacuum)
- customyielding a white powder with mp. 131-134° C.
Quellen und Nachweise
- ORD-Eintrag
- ord-2b7e6c65f7ab4df38e565224e16e81c4
- Quelldatensatz
- uspto-grants-2002_03
- Patentnummer
- US06353017B1
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