関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Bromo-3-chloropropane | HCID 8006 | — |
| 反応物 | 2-Methylbenzimidazole | HCID 11984 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 触媒 | Benzyl triethylammonium chloride | HCID 66133 | — |
| 生成物 | 1-(3-chloropropyl)-2-methyl-1H-benzimidazole | HCID 21239360 | — |
反応手順
To a stirred mixture of 13.2 parts of 2-methyl-1H-benzimidazole, 2 parts of N,N,N-triethylbenzenemethanaminium chloride and 150 parts of a sodium hydroxide solution 60% are added 30 parts of 1-bromo-3-chloropropane. To start the reaction, the whole is heated to about 40° C., whereupon the temperature rises to 50° C. (exothermic reaction). Stirring at about 50° C. is continued for 30 minutes. The reaction mixture is poured onto water and the product is extracted with methylbenzene. The extract is dried, filtered and evaporated. The residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (90:10) as eluent. The pure fractions are collected and the eluent is evaporated, yielding 1-(3-chloropropyl)-2-methyl-1H-benzimidazole as a residue.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04377578 |
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| 出典データセット | uspto-grants-1983_03 |
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| ORD ID | ord-a48a9e8a52aa4984a9662b9d83efb00a |
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| 出典メモ | uspto-grants-1983_03 |
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