Methyl iodide → HCID 67173014, compound

Participants

Reaction Steps

To a stirred solution of (±)-7-fluoro-2a,5-dihydropyrrolo[4,3,2-de]quinoline-2,4(1H,3H)-dione from Step E (608 mg, 2.95 mmol) in degassed DMF (10 mL) at 0° C. was added sodium hydride (142 mg of a 60% dispersion in mineral oil, 3.54 mmol). The mixture was stirred for 15 min, then iodomethane (0.184 mL, 2.95 mmol) was added and stirring was continued for 1 h. The reaction mixture was poured onto H2O (100 mL) and extracted with EtOAc (3×50 mL). The combined organic extracts were washed with H2O (20 mL), dried over Na2SO4, filtered, and concentrated in vacuo. The crude product was purified by silica gel chromatography, eluting with a gradient of CH2Cl2:EtOAc—100:0 to 0:100, to give the title compound. MS: m/z=221 (M+1).

Provenance & Evidence