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 | — |
反応手順
Phosphorus oxychloride (POCl3) (42.4 ml - 0.44 mole) was added to a stirred and ice-cooled solution of IV (81.2 g - 0.4 mole) in pyridine (160 ml). The temperature reached 45° C. After this addition, the mixture was heated to 60° C. The reddish-brown oil was poured immediately in 1 kg of ice/water with stirring. The precipitate was filtered, washed with ice-cold water, and dried. The crude product was crystallized from pyridine (1.5 ml/g) and water (9 ml/g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US03989522 |
|---|
| 出典データセット | uspto-grants-1976_11 |
|---|
| ORD ID | ord-f9fa9484b4744270ad3c1668120d0091 |
|---|
| 出典メモ | uspto-grants-1976_11 |
|---|