HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → (2'-Bromomethyl-6-methoxy-4'-trifluoromethyl-biphenyl-3-yl)-acetic acid methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Phosphorus tribromide | HCID 24614 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | (2'-Hydroxymethyl-6-methoxy-4'-trifluoromethyl-biphenyl-3-yl)-acetic acid methyl ester | HCID 66606415 | — |
| Solvent | 1,2-Dimethoxyethane | HCID 8071 | — |
| Product | (2'-Bromomethyl-6-methoxy-4'-trifluoromethyl-biphenyl-3-yl)-acetic acid methyl ester | HCID 66606639 | — |
Reaction Steps
To (2′-hydroxymethyl-6-methoxy-4′-trifluoromethyl-biphenyl-3-yl)-acetic acid methyl ester (1.855 g, 5.23 mmol) in DME (19 mL) was added phosphorus tribromide (0.74 mL, 7.85 mmol), and the reaction was stirred at room temperature for 1.5 hours. The mixture was cooled to 0° C., and saturated aqueous NaHCO3 and EtOAc were added. The aqueous layer was extracted with EtOAc, and the combined organic layers were dried over MgSO4, filtered, and concentrated. The residue was purified by silica gel chromatography (0-100% EtOAc in hexanes) to give the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08362044B2 |
| Source dataset | uspto-grants-2013_01 |
| ORD ID | ord-f518f89d99904d21b2361ac68f349d3d |
| Source note | uspto-grants-2013_01 |