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2,6-Difluorobenzoyl isocyanate → n-{2-[4-(3,5-Dichlorobenzyl)-3,5-diethyl-1h-pyrazol-1-yl]ethyl}-n'-(2,6-difluorobenzoyl)urea

HRID 353083
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HRID 353083 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:18]=[C:19]([Cl:21])[CH:20]=1)[CH2:5][C:6]1[C:7]([CH2:16][CH3:17])=[N:8][N:9]([CH2:13][CH2:14][NH2:15])[C:10]=1[CH2:11][CH3:12].[F:22][C:23]1[CH:33]=[CH:32][CH:31]=[C:30]([F:34])[C:24]=1[C:25]([N:27]=[C:28]=[O:29])=[O:26]>CN(C)C=O>[Cl:1][C:2]1[CH:3]=[C:4]([CH:18]=[C:19]([Cl:21])[CH:20]=1)[CH2:5][C:6]1[C:7]([CH2:16][CH3:17])=[N:8][N:9]([CH2:13][CH2:14][NH:15][C:28]([NH:27][C:25](=[O:26])[C:24]2[C:30]([F:34])=[CH:31][CH:32]=[CH:33][C:23]=2[F:22])=[O:29])[C:10]=1[CH2:11][CH3:12]
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참가 물질

4

반응물 2

HCID 27333692,6-Difluorobenzoyl isocyanateHCID 99233572-[4-(3,5-Dichlorobenzyl)-3,5-diethyl-1h-pyrazol-1-yl]ethanamine

생성물 1

HCID 10279117n-{2-[4-(3,5-Dichlorobenzyl)-3,5-diethyl-1h-pyrazol-1-yl]ethyl}-n'-(2,6-difluorobenzoyl)urea

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of the amine of Example 43 (6.5 mg, 20 μmol) in dimethylformamide (250 μL) was treated with 2,6-difluorobenzoylisocyanate (4.0 mg, 22 μmol) and the mixture was shaken for 18 hours. The reaction mixture was filtered and the filtrate was purified by HPLC (Hypersil Thermoquest Luna C8 150×10 mm column; a gradient mobile phase was used, 10:90 (by volume)→95:5 (by volume) acetonitrile:(water, 95% by volume/trifluoroacetic acid, 0.1% by volume/acetonitrile 5%, by volume)).

후처리

  1. filtrationThe reaction mixture was filtered
  2. customthe filtrate was purified by HPLC (Hypersil Thermoquest Luna C8 150×10 mm column

출처 및 근거

ORD 기록
ord-f0fb03e0fc4b4f99864d37f668882359
출처 데이터셋
uspto-grants-2004_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06750230B2

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