Methanol → HCID 22999141, compound
Reaction equation
[OH:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4]([F:11])[C:3]=1[F:12].S(=O)(=O)(O)O.[CH3:18]O>>[CH3:18][O:7][C:6](=[O:8])[C:5]1[CH:9]=[CH:10][C:2]([OH:1])=[C:3]([F:12])[C:4]=1[F:11]Participants
4
Procedure
4-hydroxy-2,3-difluoro-benzoic acid (2.0 g, 11.5 mmol) was dissolved in MeOH (20 mL) and catalytic quantity of sulfuric acid was added. The mixture was refluxed overnight, after that the solvent was evaporated under reduced pressure; the crude was dissolved in DCM and washed with saturated NaHCO3. The organic phase was dried and evaporated under reduced pressure, and the product was used without further purification.
Workup
- temperatureThe mixture was refluxed overnight
- customafter that the solvent was evaporated under reduced pressure
- dissolutionthe crude was dissolved in DCM
- washwashed with saturated NaHCO3
- customThe organic phase was dried
- customevaporated under reduced pressure
- customthe product was used without further purification
Sources & evidence
- ORD record
- ord-37ba5c0430724ddc9640e17cb6d1f7a0
- Source dataset
- uspto-grants-2012_04
- Patent number
- US08163729B2
Reaction notes
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