Acetoacetic Acid → HCID 86625997, compound

Participants

Reaction Steps

Hydrochloric acid (140 mmol, 35 mL of a 4 M solution in dioxane) was added to an ice-cooled slurry of the diacetate salt of (2-{7-[2-(4-cyanophenoxy)ethyl]-9-oxa-3,7-diazabicyclo[3.3.1]non-3-yl}ethyl)carbamic acid tert-butyl ester (10.75 g, 20 mmol; see step (i) above) in dioxane (50 mL). The reaction mixture was stirred at RT overnight. Another 65 mL (260 mmol) of 4 M HCl solution was added, after which the reaction mixture was stirred for three hours and then evaporated. The residue was dissolved in water and washed with diethyl ether. Freeze-drying of the aqueous phase gave 8.3 g (97%) the title compound as a white solid.

Provenance & Evidence