Hydrochloric Acid → HCID 22674069, compound

Participants

Reaction Steps

180 mg of white crystals were obtained using 145 mg (0.65 mmol, Production Example 5b) of 3-amino-8-bromoquinoline and 277 mg (0.85 mmol) of 1,2,3,4-tetrahydro-2-(trifluoroacetyl)isoquinoline-7-sulfonyl chloride in the same manner as in Synthetic Example 1b. Ethanol (20 ml) and an aqueous 1 N sodium hydroxide solution (0.5 ml) were added to the crystals, followed by stirring at room temperature for 30 minutes. An aqueous 1 N hydrochloric acid solution (0.4 ml) was added to the reaction solution, followed by extracting with ethyl acetate. The organic layer was washed with brine, dried over magnesium sulfate and concentrated, to give the residue. Pyridine (0.5 ml) and acetic acid anhydride (0.014 ml) were added to the residue, followed by stirring at room temperature for one hour. Brine was added thereto, followed by extracting with ethyl acetate. The organic layer was dried over magnesium sulfate and concentrated. Then, the residue was purified by silica gel chromatography, to give 113 mg of the title compound.

Provenance & Evidence