関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 2,3-Diaminotoluene | HCID 17593 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Ethyl 2-(methylamino)-2-oxoacetate | HCID 3413434 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N,4-dimethyl-1H-benzo[d]imidazole-2-carboxamide | HCID 18355052 | 37.8% |
反応手順
A mixture of 2,3-diaminotoluene (2.0 g) and ethyl N-methyloxamate (2.36 g) in N,N-dimethylformamide (10 ml) was stirred at 175° C. for 8 hours. After being cooled to ambient temperature, the mixture was poured into a mixture of saturated aqueous sodium bicarbonate solution and ethyl acetate and the organic layer was separated. The organic layer was washed with brine and the solution was dried over magnesium sulfate. The solvent was evaporated in vacuo and the residue was chromatographed on silica gel eluting with a mixture of chloroform and methanol (50:1) to give 4-methyl-2-(N-methylcarbamoyl)-1 H-benzimidazole (1.17 g) as a powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06207693B1 |
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| 出典データセット | uspto-grants-2001_03 |
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| ORD ID | ord-f9f8202b6033482b994e750c0abba420 |
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| 出典メモ | uspto-grants-2001_03 |
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