Cyclobutanol → HCID 70674457, compound

Participants

Reaction Conditions

Reaction Steps

42 mg (0.14 mmol) of bis(trichloromethyl)carbonate were added to 27.3 mg (0.38 mmol) of cyclobutanol, and the mixture was cooled to 0° C. At this temperature, 31 μl (0.38 mmol) of pyridine were added slowly, and the mixture was then stirred at 20° C. for one hour. The mixture was then cooled again to 0° C., and a solution of 100 mg (0.25 mmol) of 2-[7-(2-fluorobenzyl)imidazo[1,5-b]pyridazin-5-yl]pyrimidine-4,5,6-triamine (Example 9A) in 1 ml of pyridine was added. The reaction mixture was stirred in an ice bath for 10 minutes, and 2 ml of saturated aqueous sodium bicarbonate solution were then added. The concentrated reaction was purified by preparative HPLC (acetonitrile:water (+0.1% formic acid) gradient). This gave 25 mg (20% of theory) of the target compound.

Provenance & Evidence