Dimethylformamide → HCID 136334024、化合物

HRID 2089626ノート

反応式

HRID 2089626 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)[O:57][CH2:58][C:59]([CH3:62])([CH3:61])[CH3:60])=CC=1)([O-])=O.C(N(CC)CC)C>C(O)(=O)C>[CH3:60][C:59]([CH3:62])([CH3:61])[CH2:58][O:57][C:56](=[O:55])[N:37]=[C:36]([NH2:38])[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

6

反応物 4

HCID 6228DimethylformamideHCID 8471TriethylamineHCID 22389509Carbonic acid 2,2-dimethylpropyl ester 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 136334024HCID 136334024、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid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 (6 g) and DMF (500 mL), carbonic acid 2,2-dimethylpropyl ester 4-nitrophenyl ester [CAS No. 158810-98-1] (3.06 g) and triethylamine (4.64 mL) were added, and the resulting mixture was stirred overnight at room temperature. Acetic acid (5 mL) was added to the reaction solution, and the solvent was evaporated 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 (6.5 g).

後処理

  1. customthe solvent was evaporated 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-eeee7642280c481f937ef8f4c8be72c3
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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