Methyl iodide → HCID 117601303, compound

Participants

Reaction Steps

6-Bromo-7-methyl-4,5-dihydro-1H-benzo[b]azepin-2(3H)-one (100.0 mg, 1.998 mmol) was treated with NaH (18.9 mg, 0.472 mmol, 1.2 equiv) in DMF (3 mL) at 0° C. to room temperature for 30 min. To the mixture was added MeI (111.7 mg, 0.787 mmol, 2 equiv). The mixture was stirred at to room temperature for 1 h The mixture was quenched with water and extracted with EtOAc (30 mL×3). The organic layer was washed with brine (30 mL) and dried over Na2SO4. The solvent was removed under a reduced pressure and the crude product was purified by a silica-gel column chromatography (hexane/EtOAc 87:13 to 50:50) to give 6-bromo-1,7-dimethyl-4,5-dihydro-1H-benzo[b]azepin-2(3H)-one (88.5 mg, 83.9%).

Provenance & Evidence