Reaktionsgleichung
[N+:1]([O-:4])([O-])=[O:2].[K+].FC(F)(F)C(O)=O.[F:13][C:14]1[CH:15]=[C:16]([NH:31]C(=O)OC(C)(C)C)[CH:17]=[CH:18][C:19]=1[O:20][C:21]1[CH:22]=[N:23][C:24]([S:27]([CH3:30])(=[O:29])=[O:28])=[CH:25][CH:26]=1>>[F:13][C:14]1[C:19]([O:20][C:21]2[CH:22]=[N:23][C:24]([S:27]([CH3:30])(=[O:29])=[O:28])=[CH:25][CH:26]=2)=[CH:18][C:17]([N+:1]([O-:4])=[O:2])=[C:16]([NH2:31])[CH:15]=1Komponenten
4
Versuchsvorschrift
0.98 g of potassium nitrate was added to a trifluoroacetic acid (35 ml) solution of 3.38 g of tert-butyl (3-fluoro-4-(6-methanesulfonyl-pyridin-3-yloxy)-phenyl)-carbamate obtained in (step 2), the reaction liquid was stirred at room temperature for 1 hour, and then the solvent was evaporated away under reduced pressure. The residue was diluted with ethyl acetate, washed with aqueous saturated sodium bicarbonate and saturated saline in order, and dried with anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure, and the resulting residue was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate=1/2) to obtain the entitled compound.
Aufarbeitung
- customobtained in (step 2)
- customthe reaction liquid
- customthe solvent was evaporated away under reduced pressure
- additionThe residue was diluted with ethyl acetate
- washwashed with aqueous saturated sodium bicarbonate and saturated saline in order
- dry with materialdried with anhydrous sodium sulfate
- customThe solvent was evaporated away under reduced pressure
- customthe resulting residue was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate=1/2)
- customto obtain the entitled compound
Quellen und Nachweise
- ORD-Eintrag
- ord-90fea736829948ddbeb2e39b8bce700f
- Quelldatensatz
- uspto-grants-2010_06
- Patentnummer
- US07728025B2
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