化工社化工社 化学情報印刷レポート · 研究参考用
Sodium Carbonate → HCID 12595497、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Phenylboronic Acid | HCID 66827 | — |
| 反応物 | 2,6-Dibromoaniline | HCID 69098 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | HCID 12595497 | HCID 12595497 | 90% |
反応手順
2,6-Dibromoaniline (6.02 g, 24 mmol) and Pd(PPh3)4 (3.88 g, 3.00 mmol) were dissolved in toluene (240 ml). Phenyl boronic acid (8.80 g, 72 mmol) in EtOH (50 ml) was added. Na2CO3 (13 g, 144 mmol) in H2O (70 ml) was added. The reaction mixture was reflux for 24 hrs. The organic layer was thin separated and the amine precipitated as hydrochloride salt by addition of 20 ml of HCl. The precipitate was isolated. The salt was suspended in ether, and 2 M Na2CO3 was added. The organic layer was dried over Na2SO4 and the solvent was evaporated. The yield was 90%. 1H NMR (CDCl3): δ 7.44 (t, 4H, Harom), 7.39 (t, 4H, Harom), 7.29 (d, 2H, Harom), 7.07 (d, 2H, Harom), 6.82 (t, 1H, Harom), 3.77 (s, 2H, NH2).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07176950B2 |
| 出典データセット | uspto-grants-2007_02 |
| ORD ID | ord-32f1229f4af7448c84f5f11bab7404b8 |
| 出典メモ | uspto-grants-2007_02 |