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Sodium Azide → 3-Azido-1,3,4,5-tetrahydro-2H-1-benzazepin-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Azide | HCID 33557 | — |
| 反応物 | 3-Chloro-1,3,4,5-tetrahydro-2H-1-benzazepin-2-one | HCID 13243496 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 3-Azido-1,3,4,5-tetrahydro-2H-1-benzazepin-2-one | HCID 10932520 | — |
反応手順
A solution of 3-chloro-2,3,4,5-tetrahydro-1H-[1]benzazepin-2-one (15.9 g, 0.08 mol) and sodium azide (6.36 g, 0.10 mol) in dimethylsulfoxide (320 ml) was maintained at 80° C. under an atmosphere of nitrogen for 3 hours. At this time, the IR spectrum of an aliquot showed a strong peak at 2150 cm-1 characteristic of the azide group. The reaction mixture was poured into 1000 ml of ice/water and the suspension was stirred for 30 min. The solid was filtered off, washed with water (250 ml) and dried to give 3-azido-2,3,4,5-tetrahydro-1H-[1]benzazepin-2-one, m.p. 142°-5°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04575503 |
| 出典データセット | uspto-grants-1986_03 |
| ORD ID | ord-b3ddd47261bc4bafbec1eb97ce293cbb |
| 出典メモ | uspto-grants-1986_03 |