N-methyl-2-pyrrolidone → 2,3-Difluoro-1-(2,6-difluoro-phenoxy)-4-nitro-benzene

HRID 13334

Reaktionsgleichung

[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[OH:9].CN1CCCC1=O.[F:17][C:18]1[C:23]([F:24])=[C:22](F)[CH:21]=[CH:20][C:19]=1[N+:26]([O-:28])=[O:27]>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.C(OCC)(=O)C>[F:24][C:23]1[C:18]([F:17])=[C:19]([N+:26]([O-:28])=[O:27])[CH:20]=[CH:21][C:22]=1[O:9][C:3]1[C:2]([F:1])=[CH:7][CH:6]=[CH:5][C:4]=1[F:8]

Komponenten

Reaktionsbedingungen

Temperatur: 130 °C

Versuchsvorschrift

470 mg of 2,6-difluoro-phenol and 1.5 g of tetrabutylammonium bromide were added to an N-methylpyrrolidinone (13 ml) solution of 500 mg of 2,3,4-trifluoro-nitrobenzene, and the reaction liquid was stirred overnight at 130° C. The reaction liquid was diluted with ethyl acetate, washed with water 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=4/1) to obtain the entitled compound.

Aufarbeitung

customthe reaction liquid
customThe reaction liquid
washwashed with water 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=4/1)
customto obtain the entitled compound

Quellen und Nachweise

ORD-Eintrag: ord-11f1adab8b8e4535907931e7f083cac5
Quelldatensatz: uspto-grants-2010_06
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US07728025B2

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