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1-[({4-methyl-6'-[4-(trifluoromethyl)-1-{[2-(trimethylsilyl)ethoxy]methyl}-1H-imidazol-2-yl]-3,3'-bipyridin-6-yl}oxy)methyl]-cyclobutanecarboxylic acid → 1-[({4-methyl-6'-[5-(trifluoromethyl)-1H-imidazol-2-yl]-3,3'-bipyridin-6-yl}oxy)methyl]cyclobutanecarboxylic acid

HRID 623911
ノート
印刷プレビュー

反応式

HRID 623911 の反応式
[CH3:1][C:2]1[CH:7]=[C:6]([O:8][CH2:9][C:10]2([C:14]([OH:16])=[O:15])[CH2:13][CH2:12][CH2:11]2)[N:5]=[CH:4][C:3]=1[C:17]1[CH:18]=[N:19][C:20]([C:23]2[N:24](COCC[Si](C)(C)C)[CH:25]=[C:26]([C:28]([F:31])([F:30])[F:29])[N:27]=2)=[CH:21][CH:22]=1>FC(F)(F)C(O)=O.O>[CH3:1][C:2]1[CH:7]=[C:6]([O:8][CH2:9][C:10]2([C:14]([OH:16])=[O:15])[CH2:13][CH2:12][CH2:11]2)[N:5]=[CH:4][C:3]=1[C:17]1[CH:18]=[N:19][C:20]([C:23]2[NH:27][C:26]([C:28]([F:30])([F:29])[F:31])=[CH:25][N:24]=2)=[CH:21][CH:22]=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 679753041-[({4-methyl-6'-[4-(trifluoromethyl)-1-{[2-(trimethylsilyl)ethoxy]methyl}-1H-imidazol-2-yl]-3,3'-bipyridin-6-yl}oxy)methyl]-cyclobutanecarboxylic acid

生成物 1

HCID 679752891-[({4-methyl-6'-[5-(trifluoromethyl)-1H-imidazol-2-yl]-3,3'-bipyridin-6-yl}oxy)methyl]cyclobutanecarboxylic acid収率 86.4%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6422Trifluoroacetic acid溶媒

実験手順

In trifluoroacetic acid (3.3 mL) and water (0.33 mL) was dissolved 1-[({4-methyl-6′-[4-(trifluoromethyl)-1-{[2-(trimethylsilyl)ethoxy]methyl}-1H-imidazol-2-yl]-3,3′-bipyridin-6-yl}oxy)methyl]cyclobutanecarboxylic acid (327 mg), and the solution was stirred at room temperature for 60 hours. The reaction mixture was concentrated under reduced pressure, subjected to azeotropic distillation with acetic acid, and isopropyl ether was added to the obtained residue. The precipitated solid was collected by filtration and dried under reduced pressure to obtain 1-[({4-methyl-6′-[5-(trifluoromethyl)-1H-imidazol-2-yl]-3,3′-bipyridin-6-yl}oxy)methyl]cyclobutanecarboxylic acid (217 mg).

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. distillationsubjected to azeotropic distillation with acetic acid, and isopropyl ether
  3. additionwas added to the obtained residue
  4. filtrationThe precipitated solid was collected by filtration
  5. customdried under reduced pressure

出典と根拠

ORDレコード
ord-67ca18c5a63f4e539f4a8a1ed1dd94be
出典データセット
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09302996B2

反応ノート

読み込み中…

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