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HCID 14322382, 화합물 → HCID 11613186, 화합물

HRID 1693500
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인쇄 미리보기

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HRID 1693500 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]=[C:9](Cl)[C:10]2[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][C:11]=2[Cl:17])=[CH:4][CH:3]=1.C([O:21][C:22]([C:24]1[N:25]=[CH:26][N:27]([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)[C:28]=1[NH2:29])=O)C>ClCCCl.[Ti](Cl)(Cl)(Cl)Cl>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:22](=[O:21])[C:24]3[N:25]=[CH:26][N:27]([C:30]4[CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=4)[C:28]=3[N:29]=[C:9]2[C:10]2[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][C:11]=2[Cl:17])=[CH:4][CH:3]=1
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참가 물질

5

반응물 2

HCID 14322382HCID 14322382, 화합물HCID 57897867HCID 57897867, 화합물

생성물 1

HCID 11613186HCID 11613186, 화합물수율 36%

시약·촉매·용매 2

HCID 24193Titanium Tetrachloride촉매HCID 111,2-Dichloroethane용매

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온도
120 °C

실험 절차

To a solution of N-(4-bromo-phenyl)-2,4-dichloro-benzimidoyl chloride (0.22 mmol) and 5-amino-1-phenyl-1H-imidazole-4-carboxylic acid ethyl ester (65 mg, 0.27 mmol) in 1,2-dichloroethane is added titanium tetrachloride (98 μL, 0.89 mmol) dropwise at room temperature. After addition is completed, the reaction mixture is heated at 120° C. for 18 hours. After the reaction is quenched with water and the aqueous layer is extracted with ethyl acetate. The organic solvents are combined and dried over magnesium sulfate. Filtration and concentration provide a crude product which is purified by column chromatography gave a white solid as product (41 mg, three steps yield 36%). 1H NMR (CDCl3) δ(ppm) 8.04 (s, 1H), 7.58 (d, 2H), 7.47 (t, 2H), 7.38 (m, 3H), 7.22 (d, 1H), 7.15 (b, 1H), 7.07 (m, 2H), 6.91 (b, 1H); HPLC-MS calculated for C23H13BrCl2N40 (M+H+): 511.0. Found: 511.0.

후처리

  1. additionAfter addition
  2. customAfter the reaction is quenched with water
  3. extractionthe aqueous layer is extracted with ethyl acetate
  4. dry with materialdried over magnesium sulfate
  5. filtrationFiltration and concentration

출처 및 근거

ORD 기록
ord-7dc0a17cce1243049e840ae6b723c487
출처 데이터셋
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08158634B2

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