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N-(2-aminophenyl)-2-(1-ethyl-6-fluoro-4-hydroxy-1-H-indol-3-yl) acetamide → 3-((1H-benzo[d]imidazol-2-yl)methyl)-1-ethyl-6-fluoro-1H-indol-4-ol

HRID 1404102
ノート
印刷プレビュー

反応式

HRID 1404102 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[NH:8][C:9](=O)[CH2:10][C:11]1[C:19]2[C:14](=[CH:15][C:16]([F:21])=[CH:17][C:18]=2[OH:20])[N:13]([CH2:22][CH3:23])[CH:12]=1>C(O)(=O)C>[NH:8]1[C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=2[N:1]=[C:9]1[CH2:10][C:11]1[C:19]2[C:18]([OH:20])=[CH:17][C:16]([F:21])=[CH:15][C:14]=2[N:13]([CH2:22][CH3:23])[CH:12]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 68322751N-(2-aminophenyl)-2-(1-ethyl-6-fluoro-4-hydroxy-1-H-indol-3-yl) acetamide

生成物 1

HCID 672349353-((1H-benzo[d]imidazol-2-yl)methyl)-1-ethyl-6-fluoro-1H-indol-4-ol収率 23.9%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

The solution of 12-2 (0.3 g, 0.92 mmol) in 25 mL of acetic acid was heated to 80° C. for 8 h. The volatile was removed in vacuo and the residue was neutralized with Na2CO3 solution to pH:7. The mixture was extracted with ethyl acetate (100 mL) and washed with brine. The organic layer was dried over anhydrous Na2SO4. After filtration and concentration, a residue was obtained, which was purified by preparative TLC to give 12-3 (68 mg, 23.9%)

後処理

  1. customThe volatile was removed in vacuo
  2. extractionThe mixture was extracted with ethyl acetate (100 mL)
  3. washwashed with brine
  4. dry with materialThe organic layer was dried over anhydrous Na2SO4
  5. filtrationAfter filtration and concentration
  6. customa residue was obtained
  7. customwhich was purified by preparative TLC

出典と根拠

ORDレコード
ord-7462634bb35a4874b986e0085226df60
出典データセット
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08912220B2

反応ノート

読み込み中…

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