Carbon Dioxide → 5-Methylbenzimidazol-2-one

HRID 704450

반응식

HRID 704450 반응식
[NH2:1][C:2]1[CH:3]=[C:4]([CH3:9])[CH:5]=[CH:6][C:7]=1[NH2:8].[C:10](=O)([O-])[O-:11].[K+].[K+].C(=O)=O>O>[CH3:9][C:4]1[CH:5]=[CH:6][C:7]2=[N:8][C:10](=[O:11])[N:1]=[C:2]2[CH:3]=1

참가 물질

5

반응물 3

HCID 280Carbon Dioxide2회HCID 103323,4-DiaminotolueneHCID 11430Potassium Carbonate

생성물 1

HCID 200643865-Methylbenzimidazol-2-one수율 473.8%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
230 °C

실험 절차

24.4 g (0.2 mol) of 3,4-diaminotoluene, 18 g of water and 5.5 g (0.04 mol) of potassium carbonate were introduced into a 200 ml reactor. After sealing, CO2 was injected up to a pressure of 35 bar. The mixture was then heated to 230° C., and this temperature maintained for 12 hours. During the heating period, the pressure rose to up to 80 bar. After the reaction was completed, the mixture was cooled, the excess CO2 pressure was let down, and the aqueous slurry of crystals was removed. The aqueous catalyst solution was separated off through a filter, the solid was washed with water until it no longer contained carbonate, and was dried. 27.7 g (93.7% of theory) of 5-methylbenzimidazolone of m.p. = 301-303° C. were isolated.

후처리

  1. temperaturethis temperature maintained for 12 hours
  2. temperaturethe mixture was cooled
  3. customthe aqueous slurry of crystals was removed
  4. customThe aqueous catalyst solution was separated off through a filter
  5. washthe solid was washed with water until it no longer contained carbonate
  6. customwas dried

출처 및 근거

ORD 기록
ord-0903516235f24f02861882aaa5288405
출처 데이터셋
uspto-grants-1991_01
특허 번호
US04987234

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