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Sodium Hydroxide → 2-(2,6-dichloro-phenyl)-3H-benzoimidazole-5-carboxylic acid (3-chloro-phenyl)-methyl-amide

HRID 1514857
ノート
印刷プレビュー

反応式

HRID 1514857 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[C:9]1[NH:10][C:11]2[CH:17]=[C:16]([C:18]([OH:20])=O)[CH:15]=[CH:14][C:12]=2[N:13]=1.[CH3:21][NH:22][C:23]1[CH:28]=[CH:27][CH:26]=[C:25]([Cl:29])[CH:24]=1.F[P-](F)(F)(F)(F)F.N1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1.CCN(C(C)C)C(C)C.[OH-].[Na+]>CN(C=O)C>[Cl:29][C:25]1[CH:24]=[C:23]([N:22]([CH3:21])[C:18]([C:16]2[CH:15]=[CH:14][C:12]3[N:13]=[C:9]([C:3]4[C:2]([Cl:1])=[CH:7][CH:6]=[CH:5][C:4]=4[Cl:8])[NH:10][C:11]=3[CH:17]=2)=[O:20])[CH:28]=[CH:27][CH:26]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 14798Sodium HydroxideHCID 81531DiisopropylethylamineHCID 1389003-chloro-N-methylanilineHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 433492922-(2,6-Dichloro-phenyl)-3H-benzoimidazole-5-carboxylic acid

生成物 1

HCID 58156266
2-(2,6-dichloro-phenyl)-3H-benzoimidazole-5-carboxylic acid (3-chloro-phenyl)-methyl-amide

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 2-(2,6-dichloro-phenyl)-3H-benzoimidazole-5-carboxylic acid (107.5 mg, 0.35 mmol). N-methyl-3-chloroaniline (50 mg, 0.35 mmol), BOP (186 mg, 0.42 mmol) and DIEA (0.091 mL, 0.53 mmol) in DMF (1 mL) was stirred at room temperature for 60 h. Then 1N NaOH aqueous solution was added. The aqueous layer was extracted with EtOAc, and the organic extracts were dried over Na2SO4, filtered and concentrated under reduced pressure. The crude product was purified by column chromatography (SiO2, EtOAc:Hexane=20:80 to 80:10) and prep-HPLC later to give 2-(2,6-dichloro-phenyl)-3H-benzoimidazole-5-carboxylic acid (3-chloro-phenyl)-methyl-amide: MS (m/z) 432 (M+1); 1H NMR (CDCl3, 400 MHz) δ 9.86 (s, 1H), 7.87 (s, 1H), 7.59 (d, 1H), 7.28-7.42 (m, 4H), 7.18 (s, 1H), 7.13 (t, 2H), 6.93 (t, 1H), 3.51 (s, 3H) (major tautomer).

後処理

  1. extractionThe aqueous layer was extracted with EtOAc
  2. dry with materialthe organic extracts were dried over Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. customThe crude product was purified by column chromatography (SiO2, EtOAc:Hexane=20:80 to 80:10)

出典と根拠

ORDレコード
ord-c8a56b9c20a847d0817b6a1089057d0c
出典データセット
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08222248B2

反応ノート

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