Dimethylformamide → N-[1-amino-1-(4-{[[2-fluoro-3-(2-hydroxyethoxy)-5-methoxyphenyl]-(5-oxo-1-pyrimidin-2-yl-4,5-dihydro-1H-[1,2,4]triazol-3-yl)methyl]amino}phenyl)methylidene]-4-methylbenzamide

HRID 2089645ノート

反応式

HRID 2089645 の反応式
C(O)(=O)C.[F:5][C:6]1[C:11]([O:12][CH2:13][CH2:14][OH:15])=[CH:10][C:9]([O:16][CH3:17])=[CH:8][C:7]=1[CH:18]([NH:31][C:32]1[CH:40]=[CH:39][C:35]([C:36]([NH2:38])=[NH:37])=[CH:34][CH:33]=1)[C:19]1[NH:23][C:22](=[O:24])[N:21]([C:25]2[N:30]=[CH:29][CH:28]=[CH:27][N:26]=2)[N:20]=1.CN(C=O)C.[N+](C1C=CC([O:55][C:56](=O)[C:57]2[CH:62]=[CH:61][C:60]([CH3:63])=[CH:59][CH:58]=2)=CC=1)([O-])=O>C(N(CC)CC)C>[NH2:37][C:36](=[N:38][C:56](=[O:55])[C:57]1[CH:62]=[CH:61][C:60]([CH3:63])=[CH:59][CH:58]=1)[C:35]1[CH:34]=[CH:33][C:32]([NH:31][CH:18]([C:7]2[CH:8]=[C:9]([O:16][CH3:17])[CH:10]=[C:11]([O:12][CH2:13][CH2:14][OH:15])[C:6]=2[F:5])[C:19]2[NH:23][C:22](=[O:24])[N:21]([C:25]3[N:26]=[CH:27][CH:28]=[CH:29][N:30]=3)[N:20]=2)=[CH:40][CH:39]=1

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 532509p-Toluic acid, 4-nitrophenyl esterHCID 1363340234-({[2-fluoro-3-(2-hydroxyethoxy)-5-methoxyphenyl]-(5-oxo-1-pyrimidin-2-yl-4,5-dihydro-1H-[1,2,4]triazol-3-yl)methyl}amino)benzamidine acetic acid salt

生成物 1

HCID 136334026N-[1-amino-1-(4-{[[2-fluoro-3-(2-hydroxyethoxy)-5-methoxyphenyl]-(5-oxo-1-pyrimidin-2-yl-4,5-dihydro-1H-[1,2,4]triazol-3-yl)methyl]amino}phenyl)methylidene]-4-methylbenzamide

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

To a mixture of 4-({[2-fluoro-3-(2-hydroxyethoxy)-5-methoxyphenyl]-(5-oxo-1-pyrimidin-2-yl-4,5-dihydro-1H-[1,2,4]triazol-3-yl)methyl}amino)benzamidine acetic acid salt (1.6 g) and DMF (120 mL), 4-methylbenzoic acid 4-nitrophenyl ester [CAS No. 15023-67-3] (815 mg) and triethylamine (1.21 mL) were added, and the resulting mixture was stirred overnight at room temperature. The solvent in the reaction solution was distilled off under reduced pressure. The residue obtained was purified by NAM silica gel column chromatography (mixed solvent of methanol-ethyl acetate) to obtain the captioned compound (1.01 g).

後処理

  1. distillationThe solvent in the reaction solution was distilled off under reduced pressure
  2. customThe residue obtained
  3. customwas purified by NAM silica gel column chromatography (mixed solvent of methanol-ethyl acetate)

出典と根拠

ORDレコード
ord-7a923c9240eb4748899e8ceeccc09159
出典データセット
uspto-grants-2013_05
特許番号
US08436009B2

反応ノート

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