関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | Mls000756290 | HCID 292579 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 1-Ethyl-2-methyl-1H-benzimidazole-5-carbonitrile | HCID 722385 | 61% |
反応手順
42.4 ml (0.44 mole) of phosphorus oxychloride were added to a stirred and ice-cooled solution of 81.2 g (0.4 mole) of compound IV in 160 ml of pyridine. The temperature reached 45° C. Thereupon the mixture was heated to 60° C. The reddish-brown oil obtained was poored immediately in 1 kg of an ice-water mixture with stirring. The precipitate was filtered, washed with ice-cold water and dried. The crude product obtained was crystallized from pyridine (1.5 ml/g) and water (9 mg/g). Melting point: 162° C. Yield: 61% (452 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04062682 |
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| 出典データセット | uspto-grants-1977_12 |
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| ORD ID | ord-478948bf574d48a0a41448557b7bfbd4 |
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| 出典メモ | uspto-grants-1977_12 |
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