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Toluene → 3-(2,4-Dichlorophenyl)aniline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 3-Iodoaniline | HCID 12271 | — |
| 反応物 | (2,4-Dichlorophenyl)boronic acid | HCID 2734659 | — |
| 触媒 | Tetrakis(triphenylphosphine)palladium | HCID 11979704 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-(2,4-Dichlorophenyl)aniline | HCID 22170946 | 36.3% |
反応手順
2.0 g (10.4 mmol) of 2,4-dichlorophenylboronic acid, 2.4 g (11.0 mmol) of 3-iodoaniline, 3.2 g (30.0 mmol) of sodium carbonate and 1.6 g (1.4 mmol) of tetrakis(triphenylphosphine) palladium were added to a solvent mixture of 70 ml of toluene, 30 ml of ethanol and 30 ml of water, and the reaction was carried out under reflux with heating for 2 hours. The reaction mixture was poured into ice-cold water and extracted with toluene. The toluene layer was washed with water twice and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain 0.9 g of 3-(2,4-dichlorophenyl)aniline (yield 36.0%), which was used in Example 9 as the starting material.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07612105B2 |
| 出典データセット | uspto-grants-2009_11 |
| ORD ID | ord-1683c2d03b5f44129c2f9bbd494892a4 |
| 出典メモ | uspto-grants-2009_11 |