関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Carbon Dioxide | HCID 280 | — |
| 反応物 | 3,4-Diaminotoluene | HCID 10332 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5-Methylbenzimidazol-2-one | HCID 20064386 | 473.8% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04987234 |
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| 出典データセット | uspto-grants-1991_01 |
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| ORD ID | ord-0903516235f24f02861882aaa5288405 |
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| 出典メモ | uspto-grants-1991_01 |
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