Selectfluor → HCID 91619055, compound

Selectfluor™ (2.49 g, 7.02 mmol) was added to a solution of 7-chloro-5-fluoro-1-indanone (CAS No. 1260008-48-7, 1.08 g, 5.85 mmol) in MeOH (30 mL) at room temperature. The mixture was refluxed for 2 hours. After cooling to room temperature, the resulting mixture was evaporated to remove the solvent under reduced pressure. To the residue was added DCM and the insoluble matter was filtered off. The filtrate was concentrated in vacuo. The residue was dissolved in MeCN (20 mL) and 5 N HCl (10 mL) and the solution was stirred at room temperature for 1 hour. After concentration of the solution in vacuo, the residue was partitioned between AcOEt and H2O. The organic layer was washed with brine, dried over MgSO4, and concentrated in vacuo to afford the title compound (1.13 g, 5.58 mmol).

1. customat room temperature
2. temperatureThe mixture was refluxed for 2 hours
3. customthe resulting mixture was evaporated
4. customto remove the solvent under reduced pressure
5. additionTo the residue was added DCM
6. filtrationthe insoluble matter was filtered off
7. concentrationThe filtrate was concentrated in vacuo
8. dissolutionThe residue was dissolved in MeCN (20 mL)
9. customAfter concentration of the solution in vacuo, the residue was partitioned between AcOEt and H2O
10. washThe organic layer was washed with brine
11. dry with materialdried over MgSO4
12. concentrationconcentrated in vacuo

ORD record

ord-666284f2641a4f39ac0ad27c7896e784

Source dataset

uspto-grants-2015_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09018260B2