HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Bromo-5-nitrophenol → 5-Amino-2-trifluoromethyl-phenol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Bromo-5-nitrophenol | HCID 12867136 | — |
| Reactant | 5-Nitro-2-(trifluoromethyl)phenol | HCID 21959586 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 5-Amino-2-trifluoromethyl-phenol | HCID 15919098 | 20% |
Reaction Steps
To a solution of 5-nitro-2-(trifluoromethyl)phenol and 2-bromo-5-nitro-phenol (10 g, 48.28 mmol) in methanol (60 mL) was added Raney Nickel (2.83 g, 318 μL, 48.28 mmol) under an atmosphere of nitrogen. The reaction mixture was then stirred for 4 h at room temperature under an atmosphere of hydrogen (1 atm). The catalyst was removed by filtration through a pad of celite 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, 20%). 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).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08802700B2 |
| Source dataset | uspto-grants-2014_08 |
| ORD ID | ord-b98084b9cddb4401994aca326e6e1886 |
| Source note | uspto-grants-2014_08 |