化工社化工社 化学情報印刷レポート · 研究参考用
Ammonia → Nordiazepam
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Hexamethylenetetramine | HCID 4101 | — |
| 反応物 | 5-Chloro-2-(chloroacetamido)benzophenone | HCID 77635 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Nordiazepam | HCID 2997 | 624.3% |
反応手順
A mixture of methanol (550 mls), hexamethylenetetramine (14.1 g., 0.1 mol) and 2-chloroacetamido-5-chlorobenzophenone (308.2 g., 1.0 mol) was stirred and saturated with ammonia at room temperature. The mixture was heated slowly to reflux with a steady stream of ammonia bubbling through the solution. Refluxing was continued for 24 hours. The flow of ammonia was interrupted and the crystal slurry obtained was cooled to room temperature. The product, filtered, washed with methanol (2 × 125 ml) and hot water (4 × 500 ml), and dried gave 7-chloro-1,3-dihydro-5-phenyl-2H-1,4-benzodiazepin-2-one (169 g., 62.3%) melting at 213° to 215° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US03996209 |
| 出典データセット | uspto-grants-1976_12 |
| ORD ID | ord-57f62855293a4e2eb21841d79ab5dc2c |
| 出典メモ | uspto-grants-1976_12 |