Reaktionsgleichung
N1C=CC=CC=1.[CH3:7][C:8]([CH3:15])([C:12](Cl)=[O:13])[C:9](Cl)=[O:10].[F:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=1[CH2:23][NH:24][OH:25]>C(Cl)Cl>[F:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=1[CH2:23][N:24]1[C:9](=[O:10])[C:8]([CH3:15])([CH3:7])[C:12](=[O:13])[O:25]1Komponenten
Reaktionsbedingungen
- Temperatur
- -25 °C
Versuchsvorschrift
The procedure of Example III was utilized with 10.2 ml (0.128 mole) pyridine, 10.2 grams (0.060 mole) dimethylmalonyl chloride and 120 ml methylene chloride in solution under argon at -72° C., to which 8.5 grams (0.060 mole) of N-(2-fluorophenylmethyl)hydroxylamine (Intermediate F) in 25 ml methylene chloride was added in a single portion, raising the temperature immediately to -25° C., and stirring was continued at 0° C. for two hours. Gas chromatography on a sample of the reaction mixture showed only one major peak. The reaction mixture was washed with 2 N hydrochloric acid and water, the methylene chloride layer was separated and dried over sodium sulfate, and after removal of sodium sulfate by filtration, the solvent was removed under reduced pressure, leaving 13.0 grams of a yellow viscous liquid (91% yield). The nmr and ir spectra were consistent with the assigned structure.
Aufarbeitung
- additionwas added in a single portion
- washThe reaction mixture was washed with 2 N hydrochloric acid and water
- customthe methylene chloride layer was separated
- dry with materialdried over sodium sulfate
- customafter removal of sodium sulfate
- filtrationby filtration
- customthe solvent was removed under reduced pressure
Quellen und Nachweise
- ORD-Eintrag
- ord-6137d4825332482d92380d4b5c677f2e
- Quelldatensatz
- uspto-grants-1981_11
- Patentnummer
- US04302238
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