Sulfuric Acid → HCID 90118322, compound
Reaction equation
Cl[CH2:2][C:3]1[C:12]2[C:7](=[C:8]([F:15])[C:9]([OH:14])=[C:10]([F:13])[CH:11]=2)[O:6][C:5](=[O:16])[CH:4]=1.S(=O)(=O)(O)[OH:18]>[OH-].[Na+]>[F:13][C:10]1[C:9]([OH:14])=[C:8]([F:15])[C:7]2[O:6][CH:2]=[C:3]([CH2:4][C:5]([OH:16])=[O:18])[C:12]=2[CH:11]=1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
4-Chloromethyl-6,8-difluoro-7-hydroxy-2-chromenone (0.2 g, 0.81 mmol) obtained in Step A was dissolved in 1N NaOH aqueous solution (8 mL), and the mixture was stirred under reflux for 2 hours. The reactant was acidified by the addition of sulfuric acid, and then extracted with EtOAc. The organic layer was dried with MgSO4, and distilled under reduced pressure to obtain the title compound (0.16 g).
Workup
- temperatureunder reflux for 2 hours
- extractionextracted with EtOAc
- dry with materialThe organic layer was dried with MgSO4
- distillationdistilled under reduced pressure
Sources & evidence
- ORD record
- ord-fa832b321433472cad9a2755ba052a0b
- Source dataset
- uspto-grants-2016_09
- Patent number
- US09447044B2
Reaction notes
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