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Nitromethane → 1H-benzimidazol-1-ol 3-oxide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Nitromethane | HCID 6375 | — |
| 反応物 | 4,6-Dimethylpyrimidine | HCID 15257 | — |
| 反応物 | Benzofuroxan | HCID 68075 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1H-benzimidazol-1-ol 3-oxide | HCID 12349347 | — |
反応手順
To a mixture containing nitromethane (7.4 g., 0.12 moles), benzofuroxan 13.6 g., 0.10 moles) and tetrahydrofuran (50 ml.) is slowly added dimethylpyrimidine (11.3 g.) dropwise. The heat of reaction causes the reaction temperature to rise sharply; therefore, an ice-bath is used to maintain a steady rate of reflux. Upon completion of addition, the resulting mixture is allowed to cool to room temperature whereupon the solid product which precipitates is filtered, washed with water, dried and recrystallized from a MeOH/NaOCH3 mixture which is subsequently acidified. The crystalline product has an M.P. 213° C. dec.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04866175 |
| 出典データセット | uspto-grants-1989_09 |
| ORD ID | ord-7e53e56e1e234f45b968485bf6b00ec8 |
| 出典メモ | uspto-grants-1989_09 |