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Phenylhydrazine → N-ethyl-3,6-diformylcarbazole bis(N-phenylhydrazone)
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phenylhydrazine | HCID 7516 | — |
| 反応物 | 9-ethyl-9H-carbazole-3,6-dicarbaldehyde | HCID 3716675 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N-ethyl-3,6-diformylcarbazole bis(N-phenylhydrazone) | HCID 69210930 | — |
反応手順
Phenylhydrazine (0.2 mole, commercially available from Aldrich, Milwaukee, Wis.) and N-ethyl-3,6-diformylcarbazole (0.1 mole) were dissolved in 100 ml of a 1:1 v/v mixture of toluene and THF in 250 ml 3-neck round bottom flask equipped with a reflux condenser and a mechanical stirrer. The solution was refluxed for 2 hours. Thin layer chromatography indicated the disappearance of the starting materials. At the end of the reaction, the mixture was cooled to room temperature. The N-ethyl-3,6-diformylcarbazole bis(N-phenylhydrazone) crystals formed upon standing were filtered off, washed with isopropanol and dried in a vacuum oven at 50° C. for 6 hours. Without further purification, the product was used for the next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07090953B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-44ea98a32567491b9505acc3b6c47bd9 |
| 出典メモ | uspto-grants-2006_08 |