Carbon Dioxide → 5-Methylbenzimidazol-2-one

HRID 704450

Reaktionsgleichung

Reaktionsgleichung von HRID 704450
[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

Komponenten

5

Edukt 3

HCID 280Carbon Dioxide2×HCID 103323,4-DiaminotolueneHCID 11430Potassium Carbonate

Produkt 1

HCID 200643865-Methylbenzimidazol-2-oneAusbeute 473,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
230 °C

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-0903516235f24f02861882aaa5288405
Quelldatensatz
uspto-grants-1991_01
Patentnummer
US04987234

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