関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitrobenzene | HCID 7416 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Iodobenzene | HCID 11575 | — |
| 反応物 | 5-Aminoacenaphthene | HCID 62547 | — |
| 反応物 | N-phenyl-1,2-dihydroacenaphthylen-5-amine | HCID 1236299 | — |
| 触媒 | Copper | HCID 23978 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 5-(N,N-diphenylamino)acenaphthene | HCID 19688919 | 75.7% |
反応手順
33.85 g (0.2 mol) of 5-aminoacenaphtthene was mixed with 102.1 g (0.5 mol) of iodo benzene, 1.3 g (0.02 mol) of copper powder, 34.5 g (0.25 mol) of anhydrous potassium carbonate and 100 ml of nitrobenzene, and the mixture was stirred at 200° C. for 26 hours. The reaction was determined to be finished when disappearance of 5-aminoacenaphthene and 5-(N-phenylamino)acenaphthene as an intermediate was identified. 300 ml of toluene was added thereto to dissolve a product, and the resultant mixture was filtrated and concentrated. The concentrated product was purified by column chromatography (carrier: silica gel, eluent: toluene/hexane=1/4) to obtain 48.7 g (yield: 75.7%, melting point: 168.5°-170.5° C.) of 5-(N,N-diphenylamino)acenaphthene.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05728500 |
|---|
| 出典データセット | uspto-grants-1998_03 |
|---|
| ORD ID | ord-34a870e6034145a8adf96361ff614be2 |
|---|
| 出典メモ | uspto-grants-1998_03 |
|---|
