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Triethylamine → methyl N-({3'-fluoro-4'-[(6-fluoro-1,3-benzothiazol-2-yl)amino]biphenyl-4-yl}carbonyl)-L-valinate

HRID 2356817
ノート
印刷プレビュー

反応式

HRID 2356817 の反応式
[F:1][C:2]1[CH:3]=[C:4]([C:19]2[CH:24]=[CH:23][C:22]([C:25](O)=[O:26])=[CH:21][CH:20]=2)[CH:5]=[CH:6][C:7]=1[NH:8][C:9]1[S:10][C:11]2[CH:17]=[C:16]([F:18])[CH:15]=[CH:14][C:12]=2[N:13]=1.Cl.[CH3:29][O:30][C:31](=[O:37])[C@H:32]([CH:34]([CH3:36])[CH3:35])[NH2:33].C(N(CC)CC)C.ON1C2C=CC=CC=2N=N1.C(N=C=NC(C)C)(C)C>C(Cl)Cl.CCOC(C)=O.CN(C=O)C>[F:1][C:2]1[CH:3]=[C:4]([C:19]2[CH:24]=[CH:23][C:22]([C:25]([NH:33][C@H:32]([C:31]([O:30][CH3:29])=[O:37])[CH:34]([CH3:36])[CH3:35])=[O:26])=[CH:21][CH:20]=2)[CH:5]=[CH:6][C:7]=1[NH:8][C:9]1[S:10][C:11]2[CH:17]=[C:16]([F:18])[CH:15]=[CH:14][C:12]=2[N:13]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 8471TriethylamineHCID 12734DiisopropylcarbodiimideHCID 757711-HydroxybenzotriazoleHCID 111190Methyl valinate hydrochlorideHCID 7147096HCID 7147096、化合物

生成物 1

HCID 59009703methyl N-({3'-fluoro-4'-[(6-fluoro-1,3-benzothiazol-2-yl)amino]biphenyl-4-yl}carbonyl)-L-valinate

試薬・触媒・溶媒 3

HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

3′-Fluoro-4′-[(6-fluoro-1,3-benzothiazol-2-yl)amino]biphenyl-4-carboxylic acid (0.084 g, 0.22 mmol) and L-valine methyl ester hydrochloride (0.044 g, 0.26 mmol) were suspended in CH2Cl2 (5 mL), and triethylamine (0.04 mL, 0.26 mmol), 1-hydroxybenzotriazole (0.0296 g, 0.22 mmol), and N,N′-diisopropylcarbodiimide (0.030 mL, 0.22 mmol) were added. DMF (2.0 mL) was added to achieve dissolution, and the reaction mixture was stirred at rt overnight. The reaction mixture was diluted with EtOAc (50 mL) and was washed with water (2×50 mL) and brine (50 mL). The combined organic phases were dried over MgSO4, filtered, and concentrated in vacuo. The crude material was purified by flash column chromatography (Biotage® system; 30-40% EtOAc/Hexanes gradient). This yielded 90.4 mg (83%) of the desired product as a white solid.

後処理

  1. dissolutiondissolution
  2. washwas washed with water (2×50 mL) and brine (50 mL)
  3. dry with materialThe combined organic phases were dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe crude material was purified by flash column chromatography (Biotage® system; 30-40% EtOAc/Hexanes gradient)

出典と根拠

ORDレコード
ord-a719b61d202b46cc9249a4da68c76fea
出典データセット
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07759376B2

反応ノート

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