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

HRID 623920
ノート
印刷プレビュー

反応式

HRID 623920 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:25]2[CH:26]=[N:27][C:28]([O:32][CH2:33][C:34]3([C:38]([OH:40])=[O:39])[CH2:37][CH2:36][CH2:35]3)=[CH:29][C:30]=2[CH3:31])[CH:5]=[N:6][C:7]=1[C:8]1[N:9](COCC[Si](C)(C)C)[CH:10]=[C:11]([C:13]([F:16])([F:15])[F:14])[N:12]=1>FC(F)(F)C(O)=O.O>[Cl:1][C:2]1[CH:3]=[C:4]([C:25]2[CH:26]=[N:27][C:28]([O:32][CH2:33][C:34]3([C:38]([OH:40])=[O:39])[CH2:35][CH2:36][CH2:37]3)=[CH:29][C:30]=2[CH3:31])[CH:5]=[N:6][C:7]=1[C:8]1[NH:12][C:11]([C:13]([F:14])([F:15])[F:16])=[CH:10][N:9]=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 679753101-[({5'-chloro-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 680539781-[({5'-chloro-4-methyl-6'-[5-(trifluoromethyl)-1H-imidazol-2-yl]-3,3'-bipyridin-6-yl}oxy)methyl]cyclobutanecarboxylic acid収率 61.9%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6422Trifluoroacetic acid
溶媒

実験手順

In trifluoroacetic acid (3.1 mL) and water (0.3 mL) was dissolved 1-[({5′-chloro-4-methyl-6′-[4-(trifluoromethyl)-1-{[2-(trimethylsilyl)ethoxy]methyl}-1H-imidazol-2-yl]-3,3′-bipyridin-6-yl]oxy)methyl}cyclobutanecarboxylic acid (312 mg), and the mixture was allowed to stand at room temperature for 60 hours. The reaction mixture was concentrated under reduced pressure, subjected to azeotropic distillation with acetic acid, isopropyl ether was added to the obtained residue, and the precipitated solid was collected by filtration and dried under reduced pressure to obtain 1-[({5′-chloro-4-methyl-6′-[5-(trifluoromethyl)-1H-imidazol-2-yl]-3,3′-bipyridin-6-yl}oxy)methyl]cyclobutanecarboxylic acid (151 mg).

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. distillationsubjected to azeotropic distillation with acetic acid, 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-e2735b48436044d3b3bc66583d581abc
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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