Reaktionsgleichung
[Br:1][C:2]1[CH:10]=[CH:9][C:8]([Br:11])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[N+:12]([O-])([OH:14])=[O:13]>S(=O)(=O)(O)O>[Br:1][C:2]1[C:10]([N+:12]([O-:14])=[O:13])=[CH:9][C:8]([Br:11])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5]Komponenten
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 100 °C
Versuchsvorschrift
The procedure described in R. K. Bentley and F. G. Holliman, J. Chem Soc. (c), 2447 (1970) was used. A mixture of 2,5-dibromobenzoic acid (50 g, 0.18 mol) in concentrated sulfuric acid was vigorously stirred as fuming nitric acid (62.5 mL) was added dropwise at a rate to keep the temperature below 70° C. The reaction mixture was vigorously stirred, heated to 100° C. and then kept at 100° C. for 5 hours. The cooled reaction was cautiously poured into 2 liters of ice and vigorously stirred, the precipitate was filtered through a sintered glass funnel and the solid was washed well with water. Crystallization was achieved by dissolving the solid in acetic acid (150 mL) and after concentration to a half of the volume, crystals separated (16.72 g); mp 225-229° C. An additional crop of 7.52 g was obtained to give a total yield of 24.24 g (41%).
Aufarbeitung
- additionwas added dropwise at a rate
- customthe temperature below 70° C
- customThe cooled reaction
- stirringvigorously stirred
- filtrationthe precipitate was filtered through a sintered glass funnel
- washthe solid was washed well with water
- customCrystallization
- dissolutionby dissolving the solid in acetic acid (150 mL)
- concentrationafter concentration to a half of the volume, crystals
- customseparated (16.72 g)
- customAn additional crop of 7.52 g was obtained
- customto give a total yield of 24.24 g (41%)
Quellen und Nachweise
- ORD-Eintrag
- ord-ce703942be0f456fb61b1b178a329132
- Quelldatensatz
- uspto-grants-2000_02
- Patentnummer
- US06025380
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