HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 4-(Bromomethyl)-1-(cyclohexylmethyl)-2-(trifluoromethyl)benzene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Phosphorus tribromide | HCID 24614 | — |
| Reactant | (4-(Cyclohexylmethyl)-3-(trifluoromethyl)phenyl)methanol | HCID 67211680 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 4-(Bromomethyl)-1-(cyclohexylmethyl)-2-(trifluoromethyl)benzene | HCID 67210891 | 198.9% |
Reaction Steps
To a stirred solution of (4-(cyclohexylmethyl)-3-(trifluoromethyl)phenyl)methanol (80 mg, 0.29 mmol) in dry DCM (1 mL) was added tribromophosphine (11 μL, 0.12 mmol) at 0° C. The reaction mixture was slowly warmed to room temperature and stirred for 1 h, poured into water, extracted with DCM. The combined organics were washed with saturated NaHCO3 solution and brine, dried and concentrated. The residue was purified by column chromatography to give the title compound (80 mg) as a colorless oil. 1H NMR (400 MHz, CDCl3) δ 0.96-1.06 (m, 2H), 1.14-1.22 (m, 3H), 1.55-1.72 (m, 6H), 2.65 (d, J=6.5 Hz, 2H), 4.49 (s, 2H), 7.28 (d, J=8.0 Hz, 1H), 7.47 (dd, J=8.0 and 1.7 Hz, 1H), 7.63 (d, J=1.6 Hz, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09126932B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-118f4af649d7423d861d3cde83450fb3 |
| Source note | uspto-grants-2015_09 |