Ammonium Acetate → HCID 54285037, Verbindung
Reaktionsgleichung
[C:1]([O:10][CH2:11][C:12]([C:14]1[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][CH:15]=1)=O)(=O)[CH2:2][CH2:3][C:4]([O:6][CH2:7][CH3:8])=[O:5].C([O-])(=O)C.[NH4+:25]>C(O)(=O)C>[Cl:20][C:17]1[CH:18]=[CH:19][C:14]([C:12]2[N:25]=[C:1]([CH2:2][CH2:3][C:4]([O:6][CH2:7][CH3:8])=[O:5])[O:10][CH:11]=2)=[CH:15][CH:16]=1Komponenten
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 110 °C
Versuchsvorschrift
A mixture of 2-(4-chlorophenyl)-2-oxoethyl ethyl succinate (7.6 g), ammonium acetate (9.8 g) and acetic acid (80 ml) was stirred for an hour at 110° C. and refluxed for 2 hours. The solvent was distilled off. The residue was diluted with water, made basic by addition of aqueous sodium hydrogen carbonate solution and then extracted with ethyl acetate. The ethyl acetate layer was washed with water, and dried over MgSO4. After removal of the solvent, the oily residue was subjected to a silica gel column chromatography. Crystals of ethyl 4-(4-chlorophenyl)-2-oxazolepropionate (2.23 g, 31%) were obtained from the fraction eluted with ethyl acetate-hexane (1:3, V/V). Recrystallization from ethyl acetate-hexane gave colorless plate crystals of mp 65°-66° C.
Aufarbeitung
- temperaturerefluxed for 2 hours
- distillationThe solvent was distilled off
- additionThe residue was diluted with water
- additionmade basic by addition of aqueous sodium hydrogen carbonate solution
- extractionextracted with ethyl acetate
- washThe ethyl acetate layer was washed with water
- dry with materialdried over MgSO4
- customAfter removal of the solvent
Quellen und Nachweise
- ORD-Eintrag
- ord-b2943bded91c47d28b7c252ee3e1edda
- Quelldatensatz
- uspto-grants-1994_12
- Patentnummer
- US05371098
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