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Methacrylic Acid → 4-(N-2-hydroxyethyl-N-ethylamino)-4'-nitro-1,4-diphenyl-1,3-butadiene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methacrylic Acid | HCID 4093 | — |
| 反応物 | (4-Nitrophenyl)acetic acid | HCID 4661 | — |
| 反応物 | Aniline | HCID 6115 | — |
| 反応物 | 2-Methylbenzenesulfonic acid | HCID 6925 | — |
| 反応物 | 4-(N-2-hydroxyethyl-N-ethylamino)cinnamaldehyde | HCID 54451596 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 4-(N-2-hydroxyethyl-N-ethylamino)-4'-nitro-1,4-diphenyl-1,3-butadiene | HCID 54446572 | — |
反応手順
A solution of 21.9 g (0.1 mole) of 4-(N-2-hydroxyethyl-N-ethylamino)cinnamaldehyde, 9.3 g (1 mole) of aniline, and 0.19 g (1 mole %) of toluenesulfonic acid in toluene is heated at reflux for 17 hours with azeotropic removal of water. After the mixture is cooled to room temperature, 17.2 g (0.2 mole) of methacrylic acid and 18.1 g (0.1 mole) of 4-nitrophenylacetic acid are added to the solution, and the reaction is stirred at room temperature for 3 hours. The mixture then is heated at reflux for 16 hours. After cooling to room temperature, the solid diphenylbutadiene precipitates from solution and is collected by filtration and purified by recrystallization from ethanol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05247042 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-a7fdbb7f8cd94053be30d2daa540915e |
| 出典メモ | uspto-grants-1993_09 |