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O-Phenylenediamine → 2-(5-Methylpyridin-2-yl)benzimidazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | O-Phenylenediamine | HCID 7243 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 5-Methylpicolinic acid | HCID 199575 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-(5-Methylpyridin-2-yl)benzimidazole | HCID 20347800 | — |
反応手順
6.2 g. of o-phenylenediamine, 7.1 g. of 5-methylpicolinic acid and 40 g. of polyphosphoric acid were stirred under nitrogen gas current at 160° C. to 180° C. for 4 hours. To the reaction mixture were added 400 ml. of water and then a concentrated aqueous solution of sodium carbonate to neutrality. The resulting crystals were filtered off, dried and recrystallized from acetonitrile or ethyl acetate to obtain 9.4 g. of colorless needles of the product (86% of theory), M.P. 229.0°-229.5° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04188486 |
| 出典データセット | uspto-grants-1980_02 |
| ORD ID | ord-91f87d1198134f97a0820547c530d953 |
| 出典メモ | uspto-grants-1980_02 |