化工社化工社 化学情報印刷レポート · 研究参考用
Phosphorus pentachloride → 8,11-Dichlorodibenzo[b,f][1,4]oxazepine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phosphorus pentachloride | HCID 24819 | — |
| 反応物 | 2-Chlorodibenz(b,f)-1,4-oxazepin-11(10H)-one | HCID 76619 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 8,11-Dichlorodibenzo[b,f][1,4]oxazepine | HCID 18940415 | 89.8% |
反応手順
To a stirred solution of 8-chloro-10,11-dihydrodibenz[b,f][1,4]oxazepin-11-one (0.53 g, 2.15 mmol) in toluene (20 mL) was added phosphorus pentachloride (0.54 g, 2.58 mmol) at room temperature under argon. The resulting mixture was heated at reflux for 4 h and the solvent was removed in vacuo. The residue was redissolved in toluene and reconcentrated. The light yellow solid 8,11-dichlorodibenz[b,f][1,4]oxazepine (0.51 g, quantitative yield) was used directly for the next reaction without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05834459 |
| 出典データセット | uspto-grants-1998_11 |
| ORD ID | ord-4a7b70353d994fcf846d7799bc15809e |
| 出典メモ | uspto-grants-1998_11 |