関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzil | HCID 8651 | — |
| 反応物 | 1-(1H-benzimidazol-2-yl)guanidine | HCID 178512594 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | HCID 178420035 | HCID 178420035 | 17.8% |
反応手順
A mixture of benzil (1.05 g, 5.0 mmol) and 2-guanidinobenzimidazole (1.57 g, 9.0 mmol) in benzene (25 mL) was refluxed in pyridine (10 mL) for 1 h. After evaporating most of the pyridine under reduced pressure, the residue was treated with hot toluene and the resulting precipitate was filtered. The precipitate was then dissolved in 9:1 water:acetic acid (30 mL); the solution was filtered and the filtrate was neutralized to pH 7 with phosphate buffer. A precipitate formed, that was then collected and triturated with water to afford the title compound (0.42 g, 16%). 1H NMR (300 MHz, d6-DMSO) d 11.5 (br s, NH, 2 H), 10.0 (br s, NH, 2 H), 8.6 (br s, NH, 2 H), 7.28-7.10 (m, 14 H), 6.97 (dd, J=6.0, 3.0 Hz, 4 H); MS (ESI) m/z 525 [M+H]+; Anal. Calcd. for C30H24N10 . ½CH3CO2H ¾H2O: C, 65.37; H, 4.88; N, 24.65. Found: C, 65.36; H, 4.79; N, 24.48.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06211200B1 |
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| 出典データセット | uspto-grants-2001_04 |
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| ORD ID | ord-0ff89d8a4ec7446ea87d3fe217c44e8c |
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| 出典メモ | uspto-grants-2001_04 |
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