Reaktionsgleichung
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[NH:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[CH2:16][C:17]([OH:19])=O.[Na][Na].[NH2:22][C@H:23]([C:28]([OH:30])=[O:29])[CH2:24][C:25]([OH:27])=[O:26]>CN(C)C=O.CO.O>[Cl:8][C:4]1[CH:5]=[CH:6][CH:7]=[C:2]([Cl:1])[C:3]=1[NH:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[CH2:16][C:17]([NH:22][C@H:23]([C:28]([OH:30])=[O:29])[CH2:24][C:25]([OH:27])=[O:26])=[O:19]Komponenten
6
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Versuchsvorschrift
A solution of 3.9 g of the N-hydroxysuccinimide ester of 2-[2-(2,6-dichlorophenylamino)-phenyl]-acetic acid in dimethylformamide is added dropwise to 2.00 g of the disodium salt of L-aspartic acid in 10 ml of methanol/water (1:1). The solution is concentrated by evaporation in vacuo after one hour at room temperature, the residue is taken up in ethyl acetate and dilute hydrochloric acid and partitioned and the ethyl acetate phase is washed with water, dried with Na2SO4 and concentrated by evaporation. By trituration of the residue with diethyl ether, crystals of N-{[2-(2,6-dichlorophenylamino)-phenyl]-acetyl}-aspartic acid are obtained; m.p. 157°-160° (decomposition), Rf =0.17 (CHCl3 :MeOH=1:1).
Aufarbeitung
- concentrationThe solution is concentrated by evaporation in vacuo after one hour at room temperature
- customdilute hydrochloric acid and partitioned
- washthe ethyl acetate phase is washed with water
- dry with materialdried with Na2SO4
- concentrationconcentrated by evaporation
Quellen und Nachweise
- ORD-Eintrag
- ord-a57199d93be242c2a6e9799ef67f1707
- Quelldatensatz
- uspto-grants-1987_02
- Patentnummer
- US04640911
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