Toluene → 80854-57-5
Reaktionsgleichung
[CH3:1][C:2]([C:4]1[CH:9]=[CH:8][C:7]([N+:10]([O-:12])=[O:11])=[CH:6][CH:5]=1)=O.[C:13](C=P(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)([O:15][CH2:16][CH3:17])=[O:14].[C:38]1(C)C=CC=CC=1>>[N+:10]([C:7]1[CH:8]=[CH:9][C:4](/[C:2](/[CH3:38])=[CH:1]/[C:13]([O:15][CH2:16][CH3:17])=[O:14])=[CH:5][CH:6]=1)([O-:12])=[O:11]Komponenten
4
Versuchsvorschrift
A toluene (90 ml) solution of 4-nitroacetophenone (2.0 g) and (carbethoxymethylidene)triphenylphosphorane (6.33 g) was stirred while refluxing under heating for 10 hours. After the solution was allowed to cool, the solvent was distilled off. The obtained residue was purified by column chromatography (6.25% ethyl acetate/n-hexane) to obtain Compound 19a (829 mg, 29%) as a white solid.
Aufarbeitung
- temperaturewhile refluxing
- temperatureunder heating for 10 hours
- temperatureto cool
- distillationthe solvent was distilled off
- customThe obtained residue was purified by column chromatography (6.25% ethyl acetate/n-hexane)
Quellen und Nachweise
- ORD-Eintrag
- ord-d698436e2133487c8add22e095a73a7e
- Quelldatensatz
- uspto-grants-2010_12
- Patentnummer
- US07855300B2
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