Reaktionsgleichung
[I:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[CH3:11])[C:5]([OH:7])=[O:6].S(=O)(=O)(O)O.[CH2:17](O)[CH3:18]>>[I:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[CH3:11])[C:5]([O:7][CH2:17][CH3:18])=[O:6]Komponenten
4
Versuchsvorschrift
40.61 g of 3-iodo-4-methylbenzoic acid was suspended in 406 ml of ethanol and 9.1 ml of concentrated sulfuric acid was added, and then the mixture was heated at reflux for 24 hours. After the solvent was distilled off under reduced pressure, the residue was mixed with iced water, made basic with an aqueous saturated sodium hydrogen carbonate solution, followed by extraction with ethyl acetate twice. The extracts were washed in turn with water and saturated saline and then dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain 44.44 g of a crude product as a brown oily product.
Aufarbeitung
- temperaturethe mixture was heated
- temperatureat reflux for 24 hours
- distillationAfter the solvent was distilled off under reduced pressure
- additionthe residue was mixed with iced water
- extractionfollowed by extraction with ethyl acetate twice
- washThe extracts were washed in turn with water and saturated saline
- dry with materialdried over anhydrous magnesium sulfate
- distillationThe solvent was distilled off under reduced pressure
Quellen und Nachweise
- ORD-Eintrag
- ord-e7d713160acb4b798d7d7c899f2643a7
- Quelldatensatz
- uspto-grants-2010_06
- Patentnummer
- US07728131B2
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