Dimethylacetamide → HCID 66665839, compound

Participants

Reaction Steps

300 mg (0.54 mmol) {1-[4-(8-Bromo-6-chloro-3-phenyl-imidazo[1,2-a]pyridin-2-yl)-phenyl]-cyclobutyl}-carbamic acid tert-butyl ester, intermediate example Int-400-12, 3.5 mg (0.054 mmol) zinc, 44.3 mg (0.054 mmol) 1,1 bis(diphenylphosphino)-ferrocenedichloropalladium(II) and 127.4 mg (1.08 mmol) zinc cyanide in 4.5 mL N,N-dimethylacetamide (degassed) were heated in the microwave at 110° C. for three hours. Due to an incomplete reaction additional zinc, catalyst and zinc cyanide were added, and stirring was continued at 150° C. for one hour. The reaction mixture was diluted with ethyl acetate and washed with water/saturated ammonium chloride. The organic phase was separated, dried (sodium sulfate), filtrated and the solvent was removed. The crude product (530 mg >100%) was used in the next step without further purification.

Provenance & Evidence