化工社化工社 化学情報印刷レポート · 研究参考用
2,3,4,5-Tetrahydro-1,5-benzoxazepine → 5-Nitroso-2,3,4,5-tetrahydro-1,5-benzoxazepine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,3,4,5-Tetrahydro-1,5-benzoxazepine | HCID 577752 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5-Nitroso-2,3,4,5-tetrahydro-1,5-benzoxazepine | HCID 12233799 | 95.1% |
反応手順
To a stirred, cold slurry of 2,3,4,5-tetrahydro-1,5-benzoxazepine (13.72 g, 91.96 mmol) in 2N aqueous HCl (105 mL) was added dropwise a solution of NaNO2 (7.30 g, 105.75 mmol) in H2O (16 mL) and stirred at room temperature for 2 hrs. The mixture was taken up in H2O (800 mL), extracted with ether (3×200 mL), dried over MgSO4, and stripped of the solvent under reduced pressure to yield 15.59 g (95%) of 5-nitroso-2,3,4,5-tetrahydro-1,5-benzoxazepine as a tan powder. (M+H)+ 178.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06713471B1 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-54e9657d3fcb4bd3becb32aee40351a7 |
| 出典メモ | uspto-grants-2004_03 |