HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus tribromide → HCID 90402480, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus tribromide | HCID 24614 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 90013412 | HCID 90013412 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 90402480 | HCID 90402480 | 194.8% |
Reaction Steps
To an ice cooled solution of (±)-1-(2-chloro-3-(trifluoromethyl)phenyl)ethanol (1.1 g, 4.9 mmol) in DCM (16 mL) was added phosphorus tribromide (0.23 mL, 2.5 mmol) dropwise. The reaction was allowed to warm to rt and stirred for 3 h. Saturated aqueous NaHCO3 was added, and the mixture was extracted with DCM (×3). The combined organic extracts were dried (Na2SO4), filtered, and concentrated to give the desired product as a yellow oil (1.4 g, 97%). 1H NMR (400 MHz, CDCl3) δ 7.93-7.81 (m, 1H), 7.69-7.64 (m, 1H), 7.42 (t, J=7.9 Hz, 1H), 5.73 (q, J=7.0 Hz, 1H), 2.05 (d, J=7.0 Hz, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09040534B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-be1108faccdd469bbb62a76ac6fc2869 |
| Source note | uspto-grants-2015_05 |