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

HRID 2063603
ノート
印刷プレビュー

反応式

HRID 2063603 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 86624862HCID 86624862、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 6422Trifluoroacetic acid溶媒

実験手順

[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%.

後処理

  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)

出典と根拠

ORDレコード
ord-56a5c2c2ff0a4ec68e18b0ac24b60a70
出典データセット
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08288398B2

反応ノート

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