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

HRID 726861

반응식

HRID 726861 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 180Acetone용매HCID 962Water용매2회

실험 절차

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.

후처리

  1. filtrationthe precipitated crystalline material is filtered off with suction

출처 및 근거

ORD 기록
ord-dc58a205da50402090aa0581538f6e05
출처 데이터셋
uspto-grants-1998_01
특허 번호
US05710314

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