HuagongsheHuagongshe Chemistry Print Report · For research reference only
Boron trifluoride etherate → HCID 20258830, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Boron trifluoride etherate | HCID 8000 | — |
| Reactant | Trifluoroacetic anhydride | HCID 9845 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 2-(2-Bromophenoxy)benzoic acid | HCID 28604678 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 20258830 | HCID 20258830 | 91.8% |
Reaction Steps
To a solution of 2-(2-bromophenoxy)-benzoic acid 2j (11.8 g, 40.3 mmol) in dichloromethane (200 mL) was added trifluoroacetic anhydride (6.3 mL, 44.6 mmol), and the mixture was stirred for 30 min at rt. Boron trifluoride etherate (0.51 mL, 4.03 mmol) was added, and the mixture was stirred for 2 h at rt. The mixture was cooled in an ice bath, and a 3N sodium hydroxide solution (100 mL) was added under vigorous stirring. The organic layer was separated, washed with water and brine, dired over magnesium sulfate, filtered, and evaporated. The residue was purified over silica gel using dichloromethane as eluent. The desired fractions were collected, and evaporated to yield 10.18 g (91.8%) of title compound 3j.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07582650B2 |
| Source dataset | uspto-grants-2009_09 |
| ORD ID | ord-1054cbbaeda54899a1f653077cfc292a |
| Source note | uspto-grants-2009_09 |