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1-Bromo-3-chloropropane → 3-(3-Chloropropyl)-1,3-dihydro-7,8-dimethoxy-2H-3-benzazepin-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Bromo-3-chloropropane | HCID 8006 | — |
| 反応物 | 1,3-Dihydro-7,8-dimethoxy-2H-3-benzazepin-2-one | HCID 1482373 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 3-(3-Chloropropyl)-1,3-dihydro-7,8-dimethoxy-2H-3-benzazepin-2-one | HCID 13092503 | — |
反応手順
First 7,8-dimethoxy-1,3-dihydro-2H-3-benzazepin-2-one (131.5 g, 0.6 mol) is suspended in dimethylsulfoxide (900 ml) and mixed with potassium tert.butoxide (80.8 g, 0.72 mol) with stirring. After 10 minutes the solution obtained is added dropwise to 1-bromo-3-chloropropane (77 ml, 0.72 mol) in dimethylsulfoxide (300 ml), while cooling with ice water. After an hour the mixture is poured onto ice water. After a short time the greasy precipitate begins to crystallize. The precipitate is suction filtered, dissolved in acetone, precipitated again water water, suction filtered and dried.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04604389 |
| 出典データセット | uspto-grants-1986_08 |
| ORD ID | ord-58e2fd8bd2cd45c38ae0647325083bed |
| 出典メモ | uspto-grants-1986_08 |