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1-Hydroxybenzotriazole → N-((2-chloro-6-(trifluoromethyl)pyridin-3-yl)methyl)-2-(3-fluoro-4-(methylsulfonamidomethyl)-phenyl)propanamide

HRID 1428718
ノート
印刷プレビュー

反応式

HRID 1428718 の反応式
[Cl:1][C:2]1[C:7]([CH2:8][NH2:9])=[CH:6][CH:5]=[C:4]([C:10]([F:13])([F:12])[F:11])[N:3]=1.[F:14][C:15]1[CH:16]=[C:17]([CH:27]([CH3:31])[C:28](O)=[O:29])[CH:18]=[CH:19][C:20]=1[CH2:21][NH:22][S:23]([CH3:26])(=[O:25])=[O:24].ON1C2C=CC=CC=2N=N1.F[B-](F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2C=CC=CC=2N=N1.C(N(C(C)C)C(C)C)C>O1CCCC1.CN(C)C=O>[Cl:1][C:2]1[C:7]([CH2:8][NH:9][C:28](=[O:29])[CH:27]([C:17]2[CH:18]=[CH:19][C:20]([CH2:21][NH:22][S:23]([CH3:26])(=[O:24])=[O:25])=[C:15]([F:14])[CH:16]=2)[CH3:31])=[CH:6][CH:5]=[C:4]([C:10]([F:11])([F:12])[F:13])[N:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 72208426(2-Chloro-6-(trifluoromethyl)pyridin-3-YL)methanamineHCID 866793652-(3-Fluoro-4-(methylsulfonamidomethyl)phenyl)propanoic acid

生成物 1

HCID 86679935
N-((2-chloro-6-(trifluoromethyl)pyridin-3-yl)methyl)-2-(3-fluoro-4-(methylsulfonamidomethyl)-phenyl)propanamide
収率 61.3%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a stirred solution of (2-chloro-6-(trifluoromethyl)pyridin-3-yl)methanamine (2.9 g, 13.8 mmol) and 2-(3-fluoro-4-(methylsulfonamidomethyl)phenyl)propanoic acid (3.8 g, 13.8 mmol) in tetrahydrofuran (100 mL) were added 1-hydroxybenzotriazol (1.89 mL, 13.8 mmol), O-(1H-benzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium tetrafluoroborate (4.4 g, 13.8 mmol) and N-ethyldiisopropylamine (7 mL, 41.4 mmol) to gave an suspension. After addition of N,N-dimethylformamide (1 mL) the reaction mixture was stirred for 36 h at room temperature. The reaction mixture was concentrated under reduced pressure and the solid obtained was purified by column chromatography (silica gel: 100-200 mesh, eluent: cyclohexane/ethyl acetate 1:2) to afford N-((2-chloro-6-(trifluoromethyl)pyridin-3-yl)methyl)-2-(3-fluoro-4-(methylsulfonamidomethyl)phenyl)propanamide (3.96 g, 61%).

後処理

  1. customto gave an suspension
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. customthe solid obtained
  4. customwas purified by column chromatography (silica gel: 100-200 mesh, eluent: cyclohexane/ethyl acetate 1:2)

出典と根拠

ORDレコード
ord-efe60825561c4424b75e4f4e606abebc
出典データセット
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08937092B2

反応ノート

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