Hydrochloric Acid → HCID 68893702, compound

Participants

Reaction Steps

To a solution of the compound obtained in Example 43 (100 mg) in acetonitrile (10 ml) was added 2-chloroacetic acid amide (22 mg) and potassium carbonate (66 mg), and the mixture was stirred at room temperature for 72 hours, and at 60° C. for 6 hours. The reaction mixture was diluted with saturated sodium bicarbonate (100 ml), and extracted with ethyl acetate (50 ml) twice. The extracted solutions were combined, washed with saturated brine, dried with magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel chromatography to give a colorless amorphous substance (60 mg, 62%). To a solution of this amorphous substance (60 mg) in ethyl acetate (10 ml) was added 1 M hydrochloric acid in ether (0.5 ml), and the mixture was concentrated under reduced pressure, and purified by reprecipitation from ethanol-diethyl ether to give the title compound (42 mg) as a white powder.

Provenance & Evidence