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HCID 86624862, 화합물 → [4-(1-{[6-(2-Amino-phenyl)-2-methyl-pyrimidin-4-yl]-hydrazono}-ethyl)-phenyl]-dimethylamine

HRID 2063603
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HRID 2063603 반응식
C(OC(=O)[NH:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[C:14]1[CH:19]=[C:18]([NH:20][N:21]=[C:22]([C:24]2[CH:29]=[CH:28][C:27]([N:30]([CH3:32])[CH3:31])=[CH:26][CH:25]=2)[CH3:23])[N:17]=[C:16]([CH3:33])[N:15]=1)(C)(C)C>FC(F)(F)C(O)=O.ClCCl>[NH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[C:14]1[N:15]=[C:16]([CH3:33])[N:17]=[C:18]([NH:20][N:21]=[C:22]([C:24]2[CH:25]=[CH:26][C:27]([N:30]([CH3:32])[CH3:31])=[CH:28][CH:29]=2)[CH3:23])[CH:19]=1
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참가 물질

4

반응물 1

HCID 86624862HCID 86624862, 화합물

생성물 1

HCID 73320052[4-(1-{[6-(2-Amino-phenyl)-2-methyl-pyrimidin-4-yl]-hydrazono}-ethyl)-phenyl]-dimethylamine수율 60%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 6422Trifluoroacetic acid용매

실험 절차

[2-(6-{N′-[1-(4-dimethylamino-phenyl)-ethylidene]-hydrazino}-2-methyl-pyrimidin-4-yl)-phenyl]-carbamic acid tert-butyl ester was dissolved in 10 mL of 5% trifluoroacetic acid in dichloromethane. The resultant reaction mixture was stirred at room temperature for 2 hours before being concentrated in vacuo. The residue was dissolved in methanol and the pH was adjusted to 7 with potassium bicarbonate. After filtration the methanol was concentrated in vacuo and the residue was purified by Si gel chromatography (1:1 ethyl acetate:hexanes) yielding 140 mg (60%) of the title compound as a brown solid. HPLC Purity: 95%.

후처리

  1. customThe resultant reaction mixture
  2. concentrationbefore being concentrated in vacuo
  3. dissolutionThe residue was dissolved in methanol
  4. filtrationAfter filtration the methanol
  5. concentrationwas concentrated in vacuo
  6. customthe residue was purified by Si gel chromatography (1:1 ethyl acetate:hexanes)

출처 및 근거

ORD 기록
ord-56a5c2c2ff0a4ec68e18b0ac24b60a70
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08288398B2

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