Carbon Dioxide → 5-Methylbenzimidazol-2-one

HRID 704450

反応式

HRID 704450 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 200643865-Methylbenzimidazol-2-one収率 473.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
230 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0903516235f24f02861882aaa5288405
出典データセット
uspto-grants-1991_01
特許番号
US04987234

関連ノート

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