Hydrochloric Acid → 4-[5-(2-Chloro-4-trifluoromethylphenoxy)-2-nitrophenoxy]-3-oxo-2-(2,4-dichlorophenyl)-pentanenitrile

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Reaktionsgleichung

[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[CH2:9][C:10]#[N:11].[Li]CCCC.CCCCCC.[Cl:23][C:24]1[CH:45]=[C:44]([C:46]([F:49])([F:48])[F:47])[CH:43]=[CH:42][C:25]=1[O:26][C:27]1[CH:28]=[CH:29][C:30]([N+:39]([O-:41])=[O:40])=[C:31]([CH:38]=1)[O:32][CH:33]([CH3:37])[C:34](Cl)=[O:35].Cl>O1CCCC1>[Cl:23][C:24]1[CH:45]=[C:44]([C:46]([F:47])([F:48])[F:49])[CH:43]=[CH:42][C:25]=1[O:26][C:27]1[CH:28]=[CH:29][C:30]([N+:39]([O-:41])=[O:40])=[C:31]([CH:38]=1)[O:32][CH:33]([CH3:37])[C:34](=[O:35])[CH:9]([C:3]1[CH:4]=[CH:5][C:6]([Cl:8])=[CH:7][C:2]=1[Cl:1])[C:10]#[N:11]

Komponenten

Reaktionsbedingungen

Temperatur: -78 °C

Versuchsvorschrift

A solution of 0.93 g of 2,4-dichlorophenylacetonitrile in 30 ml of anhydrous tetrahydrofuran (hereinafter abbreviated as "THF") was cooled to -78° C. To this solution was added 3.5 ml of a 1.6Mn BuLi-hexane solution. Then, a THF solution of 2.12 g of 2-[5-(2-chloro-4-trifluoromethylphenoxy)-2-nitrophenoxy]propionic acid chloride was added thereto dropwise. The mixed solution was stirred for 30 minutes, then acidified with a 10% hydrochloric acid aqueous solution, and extracted with ethyl acetate. The ethyl acetate layer was dried over anhydrous magnesium sulfate, filtered and concentrated with a rotary evaporator.

Aufarbeitung

extractionextracted with ethyl acetate
dry with materialThe ethyl acetate layer was dried over anhydrous magnesium sulfate
filtrationfiltered
concentrationconcentrated with a rotary evaporator

Quellen und Nachweise

ORD-Eintrag: ord-67b52b8b130a4511a6c1240f92044ef8
Quelldatensatz: uspto-grants-1997_10
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US05674811

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