Chloroform → HCID 86707289, compound

Participants

Reaction Steps

Trifluoroacetic acid (1 mL) was added to a turbid solution of 2-[2-(4-tert-butylphenyl)ethyl]-N-(2,4-dimethoxybenzyl)-N-[2-fluoro-4-(4-phenylbutoxy)phenyl]-1,2,3,4-tetrahydroisoquinoline-6-sulfonamide obtained (440 mg) in anisole (5 mL) and chloroform (5 mL) while cooling in ice, and the mixture was stirred for 21 hr while cooling in ice. Saturated aqueous sodium hydrogen carbonate solution was added to the reaction mixture while cooling in ice and the mixture was extracted with ethyl acetate. The organic layer was washed with brine and dried over anhydrous magnesium sulfate and then the desiccant was filtered off, followed by concentration under reduced pressure. The resulting residue was purified by NH silica gel column chromatography (hexane:ethyl acetate=3:1→ethyl acetate only) to afford the title compound as a colorless amorphous substance (240 mg).

Provenance & Evidence