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

HRID 494408

반응식

HRID 494408 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 702Ethanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-13808874dc154a92b302c2793f31cec2
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07538140B2

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