Potassium Carbonate → 2-(2,5-dimethylphenoxymethyl)-phenylglyoxalic acid amide O-difluoromethyl oxime

HRID 726861

Reaktionsgleichung

Reaktionsgleichung von HRID 726861
[CH3:1][C:2]1[CH:23]=[CH:22][C:21]([CH3:24])=[CH:20][C:3]=1[O:4][CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[C:12](=[N:15][O:16][CH:17]([F:19])[F:18])[C:13]#[N:14].C(N)(N)=[O:26].OO.C(=O)([O-])[O-].[K+].[K+]>CC(C)=O.O>[F:19][CH:17]([F:18])[O:16][N:15]=[C:12]([C:7]1[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=1[CH2:5][O:4][C:3]1[CH:20]=[C:21]([CH3:24])[CH:22]=[CH:23][C:2]=1[CH3:1])[C:13]([NH2:14])=[O:26]

Komponenten

6

Edukt 3

HCID 11430Potassium CarbonateHCID 31294Carbamide PeroxideHCID 544049352-[2-(2,5-Dimethylphenoxymethyl)phenyl]-2-difluoromethoxyiminoacetonitrile

Produkt 1

HCID 867519722-(2,5-dimethylphenoxymethyl)-phenylglyoxalic acid amide O-difluoromethyl oxime

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 180AcetoneLösungsmittelHCID 962WaterLösungsmittel2×

Versuchsvorschrift

A solution of 4.72 g of 2-[2-(2,5-dimethylphenoxymethyl)phenyl]-2-difluoromethoxyimino-acetonitrile in 15 ml of acetone is added dropwise to a solution of 4.88 g of hydrogen peroxide-urea adduct and 0.20 g of potassium carbonate in 15 ml of water and the reaction mixture is stirred at room temperature for 16 hours. The reaction mixture is then diluted with water and the precipitated crystalline material is filtered off with suction. Chromatography on silica gel with hexane/ethyl acetate (3:1) yields pure 2-(2,5-dimethylphenoxymethyl)-phenylglyoxalic acid amide O-difluoromethyl oxime in the form of white crystals; m.p. 153°-156° C.

Aufarbeitung

  1. filtrationthe precipitated crystalline material is filtered off with suction

Quellen und Nachweise

ORD-Eintrag
ord-dc58a205da50402090aa0581538f6e05
Quelldatensatz
uspto-grants-1998_01
Patentnummer
US05710314

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