関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Acetyl chloride | HCID 6367 | — |
| 反応物 | 9-Acetyl-9H-carbazole | HCID 95837 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2,9-Diacetylcarbazole | HCID 274870 | 55.5% |
反応手順
9-Acetyl-carbazole (41.85 g, 0.2 mol) was dissolved in 1 L methylene chloride and 28.5 mL acetylchloride (0.4 mol) and 120 g aluminum chloride (0.9 mol) were added and the solution refluxed for 1.5 h. The solution was cooled to −78° C. and 6N HCl was added slowly while stirring and allowed to warm to room temperature. Methylene chloride was added to dissolve the precipitate and the solution was extracted, and the organics dried over Na2SO4, decolorized with charcoal, filtered and concentrated. Recrystallization from benzene/hexane gave 27.9 g 2,9-diacetylcarbazole.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06706753B2 |
|---|
| 出典データセット | uspto-grants-2004_03 |
|---|
| ORD ID | ord-0be714752c9d471da58ec624efb3e560 |
|---|
| 出典メモ | uspto-grants-2004_03 |
|---|
