Reaction #2120658
Related Literature (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08691804B2
Conditions: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
Procedure: To a stirred solution of 6-fluoro-3,4-dihydroisoquinolin-1(2H)-one (102 mg, 0.62 mmol) in THF (5 ml) was added NaH (49 mg of a 60% dispersion in mineral oil, 1.23 mmol) giving a thick white precipitate. After 30 minutes, methyl iodide (76 μl, 1.23 mmol) was added and the reaction was heated at 50° C. for 1 hour. Complete conversion was observed by TLC and the reaction was concentrated, diluted with dichloromethane (30 ml), washed with saturated NaHCO3 (15 ml), dried (MgSO4), filtered and concentrated in vacuo. The residue was purified by FCC (using a gradient of eluents 1:1 Hexane/EtOAc to EtOAc) to provide the title compound as colourless oil (106 mg, 96%). giving a thick white precipitate the reaction was concentrated diluted with dichloromethane (30 ml) washed with saturated NaHCO3 (15 ml) dried (MgSO4) filtered concentrated in vacuo The residue was purified by FCC (
Source ID: ord-bd2597377b964b1bb91c54de3df53c43