N-cyclopropyl-1-{4-[(ethylamino)carbonyl]phenyl}-5-[(E)-2-(1-trityl-1H-imidazol-2-yl)vinyl]-1H-1,2,3-triazole-4-carboxamide → N-cyclopropyl-1-{4-[(ethylamino)carbonyl]phenyl}-5-[(E)-2-(1H-imidazol-2-yl)vinyl]-1H-1,2,3-triazole-4-carboxamide

HRID 1717373ノート

反応式

HRID 1717373 の反応式
[CH:1]1([NH:4][C:5]([C:7]2[N:8]=[N:9][N:10]([C:38]3[CH:43]=[CH:42][C:41]([C:44]([NH:46][CH2:47][CH3:48])=[O:45])=[CH:40][CH:39]=3)[C:11]=2/[CH:12]=[CH:13]/[C:14]2[N:15](C(C3C=CC=CC=3)(C3C=CC=CC=3)C3C=CC=CC=3)[CH:16]=[CH:17][N:18]=2)=[O:6])[CH2:3][CH2:2]1>FC(F)(F)C(O)=O>[CH:1]1([NH:4][C:5]([C:7]2[N:8]=[N:9][N:10]([C:38]3[CH:39]=[CH:40][C:41]([C:44]([NH:46][CH2:47][CH3:48])=[O:45])=[CH:42][CH:43]=3)[C:11]=2/[CH:12]=[CH:13]/[C:14]2[NH:18][CH:17]=[CH:16][N:15]=2)=[O:6])[CH2:2][CH2:3]1

参加物

3

反応物 1

HCID 68513554N-cyclopropyl-1-{4-[(ethylamino)carbonyl]phenyl}-5-[(E)-2-(1-trityl-1H-imidazol-2-yl)vinyl]-1H-1,2,3-triazole-4-carboxamide

生成物 1

HCID 136104428N-cyclopropyl-1-{4-[(ethylamino)carbonyl]phenyl}-5-[(E)-2-(1H-imidazol-2-yl)vinyl]-1H-1,2,3-triazole-4-carboxamide収率 53.2%

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

N-Cyclopropyl-1-{4-[(ethylamino)carbonyl]phenyl}-5-[(E)-2-(1-trityl-1H-imidazol-2-yl)vinyl]-1H-1,2,3-triazole-4-carboxamide (670 mg) obtained in Example 322a) was dissolved in trifluoroacetic acid (5 ml), and the mixture was stirred at room temperature for 30 min. The reaction mixture was concentrated under reduced pressure, and the obtained residue was dissolved in chloroform. This chloroform solution was washed with saturated aqueous sodium hydrogen carbonate solution and saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The obtained residue was purified by basic silica gel column (ethyl acetate to ethyl acetate/methanol=4/1) to give the title compound as a white powder (220 mg).

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. dissolutionthe obtained residue was dissolved in chloroform
  3. washThis chloroform solution was washed with saturated aqueous sodium hydrogen carbonate solution and saturated aqueous sodium chloride solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe obtained residue was purified by basic silica gel column (ethyl acetate to ethyl acetate/methanol=4/1)

出典と根拠

ORDレコード
ord-300c8e3a9b84462b967510b191af0c1d
出典データセット
uspto-grants-2010_09
特許番号
US07803822B2

反応ノート

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