2-hydrazinyl-1-methyl-1H-1,3-benzodiazole → 1-(3-Isoquinolinyl)-1-ethanone-1-(1-methyl-1H-benzo[d]imidazol-2-yl)-hydrazone

HRID 2216941

反応式

HRID 2216941 の反応式
[C:1]([C:4]1[N:5]=[CH:6][C:7]2[C:12]([CH:13]=1)=[CH:11][CH:10]=[CH:9][CH:8]=2)(=O)[CH3:2].[CH3:14][N:15]1[C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=2[N:17]=[C:16]1[NH:24][NH2:25]>CO.C(O)(=O)C>[CH3:14][N:15]1[C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=2[N:17]=[C:16]1[NH:24][N:25]=[C:1]([C:4]1[N:5]=[CH:6][C:7]2[C:12]([CH:13]=1)=[CH:11][CH:10]=[CH:9][CH:8]=2)[CH3:2]

参加物

5

反応物 2

HCID 15222652-hydrazinyl-1-methyl-1H-1,3-benzodiazoleHCID 112752751-(Isoquinolin-3-yl)ethan-1-one

生成物 1

HCID 3966001-(3-Isoquinolinyl)-1-ethanone-1-(1-methyl-1H-benzo[d]imidazol-2-yl)-hydrazone

試薬・触媒・溶媒 2

HCID 176Acetic Acid触媒HCID 887Methanol溶媒

実験手順

A mixture of 3-acetylisoquinoline (1.01 g, 5.9 mmol) and 1-methyl-2-hydrazinobenzimidazole (0.96 g, 5.55 mmol) in 15 ml of methanol is stirred for approximately 7 days at room temperature after the addition of 5 drops of glacial acetic acid. The reaction is monitored by means of thin layer chromatography (Polygram Sil G/UV254 prefabricated foils; eluting agent: petroleum ether:ethyl acetate (3:7)). The reaction mixture is stored over night in the freezer at approximately −20° C. The precipitate is filtered, washed with ether and dried. The product is recrystallized from a mixture of ethylacetate and petroleum ether. Yield: 1.66 g (95% of theory).

後処理

  1. washThe reaction is monitored by means of thin layer chromatography (Polygram Sil G/UV254 prefabricated foils; eluting agent: petroleum ether:ethyl acetate (3:7))
  2. waitThe reaction mixture is stored over night in the freezer at approximately −20° C
  3. filtrationThe precipitate is filtered
  4. washwashed with ether
  5. customdried
  6. customThe product is recrystallized from a mixture of ethylacetate and petroleum ether

出典と根拠

ORDレコード
ord-c6fee03aebd242f09f4ca43a817170d2
出典データセット
uspto-grants-2006_09
特許番号
US07112680B2

関連ノート

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