Reaktionsgleichung
[Cl:1][C:2]1[C:3]([F:20])=[C:4]([CH:6]=[C:7]([Cl:19])[C:8]=1[O:9][C:10]([F:18])([F:17])[CH:11]([F:16])[C:12]([F:15])([F:14])[F:13])[NH2:5].[F:21][C:22]1[CH:32]=[CH:31][CH:30]=[C:29]([F:33])[C:23]=1[C:24]([N:26]=[C:27]=[O:28])=[O:25]>ClCCCl.ClC(Cl)C>[Cl:1][C:2]1[C:3]([F:20])=[C:4]([NH:5][C:27]([NH:26][C:24](=[O:25])[C:23]2[C:29]([F:33])=[CH:30][CH:31]=[CH:32][C:22]=2[F:21])=[O:28])[CH:6]=[C:7]([Cl:19])[C:8]=1[O:9][C:10]([F:17])([F:18])[CH:11]([F:16])[C:12]([F:14])([F:15])[F:13]Komponenten
Reaktionsbedingungen
- Temperatur
- 40 °C
Versuchsvorschrift
To a solution of 1.31 g 3,5-dichloro-2-fluoro-4-(1,1,2,3,3,3-hexafluoropropoxy) aniline in 5 mL 1,2-dichloroethane under an atmosphere of nitrogen at room temperature was added 0.87 g 2,6-difluorobenzoyl isocyanate dissolved in 10 mL dichloroethane dropwise over a 10 minute period. The mixture was stirred, warmed to 40° C. for a one hour period, then concentrated under vacuum to a brown solid 2.0 g. The mixture was chromatographed using a Michel-Miller low pressure silica gel column eluted with 4:1 dichloromethane/heptane. Like fractions were pooled and concentrated under vacuum to give 1.67 g of a light tan solid, mp 156°-7° C. Proton and 19F nmr spectra were consistent with the proposed structure. Anal. calcd C17H7Cl2F9N2O3 : C, 38.58; H, 1.33; N, 5.29. Found: C, 38.64; H, 1.40; N, 5.44.
Aufarbeitung
- concentrationconcentrated under vacuum to a brown solid 2.0 g
- customThe mixture was chromatographed
- washeluted with 4:1 dichloromethane/heptane
- concentrationconcentrated under vacuum
Quellen und Nachweise
- ORD-Eintrag
- ord-517f917d2e8049cbb917c0d1735f693f
- Quelldatensatz
- uspto-grants-1999_03
- Patentnummer
- US05886221
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