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2-Cyclopropanecarbonylpyridine → N-[(Z)-[cyclopropyl(pyridin-2-yl)methylidene]amino]-1-methylbenzimidazol-2-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Cyclopropanecarbonylpyridine | HCID 576289 | — |
| 反応物 | 2-hydrazinyl-1-methyl-1H-1,3-benzodiazole | HCID 1522265 | — |
| 触媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | N-[(Z)-[cyclopropyl(pyridin-2-yl)methylidene]amino]-1-methylbenzimidazol-2-amine | HCID 140461904 | — |
反応手順
A mixture of cyclopropyl-(2-pyridyl)-methanone (1,00 g, 7,40 mmol) and 1-methyl-2-hydrazinobenzimidazole (1.20 g, 7.40 mmol) in 20 ml of methanol is stirred for 3 days at room temperature after the addition of 6 drops of glacial acetic acid. Monitoring is effected by means of thin layer chromatography (Polygram Sil G/UV254 prefabricated foils; eluting agent: CH2Cl2:MeOH (12:1)). Subsequently, the reaction mixture is diluted with distilled water until a precipitate forms and stored in the refrigerator at approximately 5° C. for 24 hours. The precipitate is filtered, washed several times with 50% methanol, and dried. The product is recrystallized from a mixture of methanol and water. Yield: 0.97 g (45% of theory).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07112680B2 |
| 出典データセット | uspto-grants-2006_09 |
| ORD ID | ord-33d97b1198784fbe8bfd770cbe9bb30a |
| 出典メモ | uspto-grants-2006_09 |