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3-Chloropropionyl chloride → 9-(3-Chloropropionyl)-1,2,3,4,4a,9a-hexahydrocarbazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Chloropropionyl chloride | HCID 69364 | — |
| 反応物 | 2,3,4,4a,9,9a-Hexahydro-1H-carbazole | HCID 101162 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 9-(3-Chloropropionyl)-1,2,3,4,4a,9a-hexahydrocarbazole | HCID 18971610 | 111.7% |
反応手順
To a solution of 10 g 1,2,3,4,4a,9a-hexahydrocarbazole in 30 ml acetone was added a solution of 8.3 g 3-chloropropionyl chloride in 30 ml acetone dropwise at ambient temperature and the mixture was refluxed for 1 hour. The solvent was then distilled off under reduced pressure and the residue was dissolved in 100 ml of dichloromethane and washed with 10% hydrochloric acid twice. The solution was dried over anhydrous sodium sulfate and the solvent was distilled off under reduced pressure to provide about 17 g of 9-(3-chloropropionyl)-1,2,3,4,4a,9a-hexahydrocarbazole as a viscous oil. This oil was not purified but submitted directly to the next reaction.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05620973 |
| 出典データセット | uspto-grants-1997_04 |
| ORD ID | ord-49efc3352c18409b82cd5e0c284e7385 |
| 出典メモ | uspto-grants-1997_04 |