HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 1,1,1-Trifluoro-2-(4-methoxyphenyl)propan-2-ol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 4-Bromoanisole | HCID 7730 | — |
| Reactant | Methyl trifluoromethyl ketone | HCID 9871 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 1,1,1-Trifluoro-2-(4-methoxyphenyl)propan-2-ol | HCID 10867787 | — |
Reaction Steps
A solution of 1-bromo-4-methoxybenzene (19 ml, 150 mmol) in 300 ml of dry THF at −78° C. was treated with n-butyllithium (96 ml, 154 mmol) (1.6 M or 15% in hexanes, Strem). The resulting mixture was stirred for an additional 30 min. At −78° C., 1,1,1-trifluoropropan-2-one (16 ml, 180 mmol) was added and the mixture was stirred −78° C. and slowly warmed up overnight. The reaction mixture was treated with 100 ml of 5N HCl and concentrated. The layers were separated. The bottom layer (organic) was diluted with 50 ml of DCM, washed with 1×100 ml of H2O, and dried (MgSO4) and concentrated to give an oil which was purified by silica gel chromatography eluting with 0-5% EtOAc in hexanes to provide the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08552181B2 |
| Source dataset | uspto-grants-2013_10 |
| ORD ID | ord-22992592b82d45858ab498a33b94d51b |
| Source note | uspto-grants-2013_10 |