HuagongsheHuagongshe Chemistry Print Report · For research reference only
Boron trifluoride etherate → 3-Bromo-9H-xanthen-9-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Boron trifluoride etherate | HCID 8000 | — |
| Reactant | Trifluoroacetic anhydride | HCID 9845 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 4-Bromo-2-phenoxybenzoic acid | HCID 23053920 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 3-Bromo-9H-xanthen-9-one | HCID 231608 | 96.7% |
Reaction Steps
To a suspension of 4-bromo-2-phenoxy-benzoic acid (35.1 g, 120 mmol) in CH2Cl2 (350 mL) at 0° C. was added trifluoroacetic anhydride (20.3 mL, 144 mmol), dropwise, and the reaction was stirred for 15 min. At that time, boron trifluoride diethyl etherate (1.46 mL, 12.0 mmol) was added, dropwise. The reaction became homogeneous upon stirring for 1 h at room temperature. Upon completion, the reaction was poured into 1 N NaOH, and the organic phase was dried over magnesium sulfate, filtered, and concentrated to give Compound 3a (32.14 g, 116 mmol). MS m/z (MH+) 275.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07589103B2 |
| Source dataset | uspto-grants-2009_09 |
| ORD ID | ord-875eab9e6cd74fc7af06c24e010acd41 |
| Source note | uspto-grants-2009_09 |