化工社化工社 化学情報印刷レポート · 研究参考用
2-Bromo-5-nitrophenol → 5-Amino-2-trifluoromethyl-phenol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Bromo-5-nitrophenol | HCID 12867136 | — |
| 反応物 | 5-Nitro-2-(trifluoromethyl)phenol | HCID 21959586 | — |
| 触媒 | Nickel | HCID 935 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 5-Amino-2-trifluoromethyl-phenol | HCID 15919098 | 11% |
反応手順
To a solution of 5-nitro-2-(trifluoromethyl)phenol and 2-bromo-5-nitrophenol (10 g, crude) in MeOH (60 mL) was added Raney Ni (2 g) under an atmosphere of nitrogen. The mixture was stirred under hydrogen atmosphere (1 atm) at r. t. for 4 h. The catalyst was filtered off through the celite pad and the filtrate was evaporated under vacuum. The crude product was purified by preparative HPLC to obtain 5-amino-2-(trifluoromethyl)phenol (1.7 g, 11% yield for 3 steps). 1H-NMR (400 MHz, DMSO-d6) δ 9.79 (s, 1H), 7.04 (d, J=8.8 Hz, 1H), 6.10 (s, 1H), 6.01 (d, J=8.4 Hz, 1H), 5.58 (br s, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08633189B2 |
| 出典データセット | uspto-grants-2014_01 |
| ORD ID | ord-3aacce145daa4f7c83cc6d2e2595fa89 |
| 出典メモ | uspto-grants-2014_01 |