関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Ammonium Hydroxide | HCID 14923 | — |
| 反応物 | Sodium Azide | HCID 33557 | — |
| 反応物 | Chromanone | HCID 68110 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2,3,4,5-Tetrahydro-1,4-benzoxazepin-5-one | HCID 340629 | — |
反応手順
To 4-chromanone (50 g, 340 mmol) in acetic acid (670 ml) was added sodium azide (66.31 g, 1.02 mol) and conc. sulfuric acid (100 ml) dropwise at 0° C. The mixture was heated to 50° C. for 4 h and then cooled to room temperature. The mixture was poured onto ice (1 l) and basified with conc. ammonium hydroxide. The mixture was stirred for 24 h and the solids were collected by filtration (30.43 g, 55%), MSm/z 164 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06489322B1 |
|---|
| 出典データセット | uspto-grants-2002_12 |
|---|
| ORD ID | ord-03f9efa86db84893bb5663712dff59b7 |
|---|
| 出典メモ | uspto-grants-2002_12 |
|---|
