Acetylacetone → 2-Methyl-4-nitro-1H-benzo[d]imidazole

HRID 494408

反応式

HRID 494408 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([NH2:10])[C:5]=1[NH2:11])([O-:3])=[O:2].[CH3:12][C:13](=O)CC(=O)C>C(O)C.Cl>[CH3:12][C:13]1[NH:10][C:6]2[CH:7]=[CH:8][CH:9]=[C:4]([N+:1]([O-:3])=[O:2])[C:5]=2[N:11]=1

参加物

5

反応物 2

HCID 31261AcetylacetoneHCID 43595253-Nitro-1,2-phenylenediamine

生成物 1

HCID 15126612-Methyl-4-nitro-1H-benzo[d]imidazole収率 95.1%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 702Ethanol溶媒

実験手順

3-Nitrobenzene-1,2-diamine (1.0 g) was dissolved in ethanol (90 mL) and 5N hydrochloric acid (24 mL), and to this solution was added 2,4-pentanedione (1.3 g). The mixture was heated for 3 hours under reflux, cooled down to room temperature and concentrated. To this concentrate was added ethyl acetate, and the mixture was washed successively with saturated aqueous sodium bicarbonate and water, and dried over sodium sulfate to give the title compound (1.1 g).

後処理

  1. temperatureThe mixture was heated for 3 hours
  2. temperatureunder reflux
  3. concentrationconcentrated
  4. additionTo this concentrate was added ethyl acetate
  5. washthe mixture was washed successively with saturated aqueous sodium bicarbonate and water
  6. dry with materialdried over sodium sulfate

出典と根拠

ORDレコード
ord-13808874dc154a92b302c2793f31cec2
出典データセット
uspto-grants-2009_05
特許番号
US07538140B2

関連ノート

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