Reaktionsgleichung
C([O:3][C:4](=[O:15])[C:5]([C:7]1[S:8][C:9]([Br:14])=[C:10]([Br:13])[C:11]=1[Br:12])=[O:6])C.Cl>CC(C)=O.O>[Br:12][C:11]1[C:10]([Br:13])=[C:9]([Br:14])[S:8][C:7]=1[C:5](=[O:6])[C:4]([OH:15])=[O:3]Komponenten
5
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Versuchsvorschrift
A solution of (3,4,5-tribromothiophen-2-yl)-oxo-acetic acid ethyl ester (0.4 g, 0.95 mmol) in acetone (10 ml), water (2 ml), and conc. HCl (8 ml) was stirred under reflux for 1.5 hours. The reaction mixture was allowed to cool to ambient temperature and concentrated in vacuo to remove acetone which gave rise to solids which were collected, washed with water and dried. (3,4,5-tribromothiophen-2-yl)-oxo-acetic acid was thus obtained as a light yellow solid (0.17 g, 49%). MS (M−H)−: 392.75; 13C NMR (75 MHz, CDCl3) δ124.19, 117.80, 113.26, 111.72. IR (KBr) cm−1 3477.9, 3107.1, 2922.5, 1715.9, 1681.5, 1666.0, 1484.5, 1306.5, 1268.9.
Aufarbeitung
- temperatureunder reflux for 1.5 hours
- concentrationconcentrated in vacuo
- customto remove acetone which
- customgave rise to solids which
- customwere collected
- washwashed with water
- customdried
Quellen und Nachweise
- ORD-Eintrag
- ord-bd26dfa5677b41c5bf4baec1fcf716b3
- Quelldatensatz
- uspto-grants-2003_09
- Patentnummer
- US06613786B2
Verknüpfte Notizen
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