2-(5-(2-(Aminomethyl)-4-fluorophenoxy)-1H-indazol-1-yl)ethanol → 1-((5-fluoro-2-(1-(2-hydroxyethyl)-1H-indazol-5-yloxy)phenyl)methyl)-3-(3-(1-hydroxy-2-methylpropan-2-yl)-1-p-tolyl-1H-pyrazol-5-yl)urea

HRID 220221ノート

反応式

HRID 220221 の反応式
[OH:1][CH2:2][C:3]([C:6]1[CH:10]=[C:9]([NH:11][C:12](=[O:19])OCC(Cl)(Cl)Cl)[N:8]([C:20]2[CH:25]=[CH:24][C:23]([CH3:26])=[CH:22][CH:21]=2)[N:7]=1)([CH3:5])[CH3:4].[NH2:27][CH2:28][C:29]1[CH:47]=[C:46]([F:48])[CH:45]=[CH:44][C:30]=1[O:31][C:32]1[CH:33]=[C:34]2[C:38](=[CH:39][CH:40]=1)[N:37]([CH2:41][CH2:42][OH:43])[N:36]=[CH:35]2>CC(N(C)C)=O>[F:48][C:46]1[CH:45]=[CH:44][C:30]([O:31][C:32]2[CH:33]=[C:34]3[C:38](=[CH:39][CH:40]=2)[N:37]([CH2:41][CH2:42][OH:43])[N:36]=[CH:35]3)=[C:29]([CH2:28][NH:27][C:12]([NH:11][C:9]2[N:8]([C:20]3[CH:21]=[CH:22][C:23]([CH3:26])=[CH:24][CH:25]=3)[N:7]=[C:6]([C:3]([CH3:5])([CH3:4])[CH2:2][OH:1])[CH:10]=2)=[O:19])[CH:47]=1

参加物

4

反応物 2

HCID 445421222-(5-(2-(Aminomethyl)-4-fluorophenoxy)-1H-indazol-1-yl)ethanolHCID 445422572,2,2-Trichloroethyl 3-(1-hydroxy-2-methylpropan-2-yl)-1-p-tolyl-1H-pyrazol-5-ylcarbamate

生成物 1

HCID 252074011-((5-fluoro-2-(1-(2-hydroxyethyl)-1H-indazol-5-yloxy)phenyl)methyl)-3-(3-(1-hydroxy-2-methylpropan-2-yl)-1-p-tolyl-1H-pyrazol-5-yl)urea収率 50.9%

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

実験手順

2,2,2-Trichloroethyl 3-(1-hydroxy-2-methylpropan-2-yl)-1-p-tolyl-1H-pyrazol-5-ylcarbamate (0.010 g, 0.024 mmol) was added to a minimal amount of DMA, 2-(5-(2-(Aminomethyl)-4-fluorophenoxy)-1H-indazol-1-yl)ethanol (prepared in steps E1-E6; 0.0079 g, 0.026 mmol) and DEA (0.0084 mmol, 0.048 mmol) were added, and the reaction mixture was stirred at ambient temperature overnight. The reaction mixture was concentrated to remove the majority of DMA. The residue was purified by silica gel chromatography using 5% MeOH in ethyl acetate to provide 7 mg of the title compound. MS M+1 (573).

後処理

  1. additionwere added
  2. concentrationThe reaction mixture was concentrated
  3. customto remove the majority of DMA
  4. customThe residue was purified by silica gel chromatography

出典と根拠

ORDレコード
ord-73515eb8ae274f5584d43f63158bf037
出典データセット
uspto-grants-2012_06
特許番号
US08202899B2

反応ノート

読み込み中…