HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → 5-Amino-2-fluorophenol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Boron tribromide | HCID 25134 | — |
| Reactant | 4-Fluoro-3-methoxyaniline | HCID 2774533 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 5-Amino-2-fluorophenol | HCID 22641413 | 73% |
Reaction Steps
To a mixture of 4-fluoro-3-methoxyaniline (2.0 g, 14.2 mmol) in CH2Cl2 (20 mL) at 0° C. was added 1.0 M solution of BBr3 in CH2Cl2 (40 mL). It was stirred overnight, at which time the temperature was raised to room temperature. To it was added MeOH and the solvents were removed under reduced pressure. To the residue was added water, basified with saturated NaHCO3, and extracted with EtOAc. Extracts were washed with brine, dried over MgSO4, and concentrated under reduced pressure to afford 5-amino-2-fluorophenol as solid (1.3 g, 73%). 1H NMR (300 MHz, DMSO-d6) δ 9.26 (s, 1H), 6.81 (dd, 1H), 6.34 (dd, 1H), 6.04 (dd, 1H), 4.63 (br, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09320739B2 |
| Source dataset | uspto-grants-2016_04 |
| ORD ID | ord-bcc200eb084f4560a9d25c7dbb714f4d |
| Source note | uspto-grants-2016_04 |