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Methanol → 3-(5-(4-Chlorophenyl)-1-(2,4-dichlorophenyl)-4-methyl-1H-pyrazol-3-yl)-5-cyclopentyl-1H-1,2,4-triazole

HRID 254829
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HRID 254829 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:12]([C:13]3[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:14]=3[Cl:20])[N:11]=[C:10]([C:21]#[N:22])[C:9]=2[CH3:23])=[CH:4][CH:3]=1.[CH:24]1([C:29]([NH:31][NH2:32])=O)[CH2:28][CH2:27][CH2:26][CH2:25]1.C(=O)([O-])[O-].[K+].[K+].CO>C(O)CCC>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[N:12]([C:13]3[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:14]=3[Cl:20])[N:11]=[C:10]([C:21]3[N:22]=[C:29]([CH:24]4[CH2:28][CH2:27][CH2:26][CH2:25]4)[NH:31][N:32]=3)[C:9]=2[CH3:23])=[CH:6][CH:7]=1
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참가 물질

6

반응물 4

HCID 887MethanolHCID 11430Potassium CarbonateHCID 240040CyclopentanecarbohydrazideHCID 668444145-(4-chloro phenyl)-1-(2,4-dichlorophenyl)-4-methyl-1H-pyrazole-3-carbonitrile

생성물 1

HCID 248103323-(5-(4-Chlorophenyl)-1-(2,4-dichlorophenyl)-4-methyl-1H-pyrazol-3-yl)-5-cyclopentyl-1H-1,2,4-triazole

시약·촉매·용매 1

HCID 263
1-Butanol
용매

실험 절차

A solution of 5-(4-chlorophenyl)-1-(2,4-dichlorophenyl)-4-methyl-1H-pyrazole-3-carbonitrile (300 mg, 0.83 mmol), cyclopentanecarbohydrazide (116 mg, 0.90 mmol) and potassium carbonate (57 mg, 0.41 mmol) dissolved in 1-butanol (2 ml) was placed in a sealed tube, stirred at room temperature for 10 minutes and then refluxed at 150° C. for 1 day. The mixture was cooled down to room temperature and methanol (4 ml) was added thereto, followed by filtering. The filtrate was purified by reverse phase preparative HPLC, to obtain the title compound as white solid.

후처리

  1. customwas placed in a sealed tube
  2. temperaturerefluxed at 150° C. for 1 day
  3. temperatureThe mixture was cooled down to room temperature
  4. filtrationby filtering
  5. customThe filtrate was purified by reverse phase preparative HPLC

출처 및 근거

ORD 기록
ord-6a40cbd8791844e59d509ce09792e693
출처 데이터셋
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07875647B2

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