Ethyl Acetate → HCID 86702540, compound

Participants

Reaction Conditions

Reaction Steps

150 mg (0.26 mmol) {1-[4-(7-Bromo-3-phenylpyrimido[1,2-b]indazol-2-yl)phenyl]-cyclobutyl}carbamic acid tert-butyl ester (intermediate example Int-2-1), 1.7 mg (0.026 mmol) zinc, 21.6 mg (0.026 mmol) bis(diphenylphosphino)ferrocenedichloropalladium(II) and 61.8 mg (0.53 mmol) zinc cyanide in 2.2 mL N,N-dimethylacetamide, (degassed) were stirred in the microwave for four hours at 110° C. After addition of a further equivalent of zinc cyanide and a spatelspitze of zinc and bis(diphenylphosphino)ferrocenedichloropalladium(II) stirring was continued for three hours at 110° C. Despite an incomplete reaction the mixture was worked up. After addition of ethyl acetate the organic phase was washed twice with water and saturated ammonium chloride, dried over sodium sulfate, filtrated, and the solvent was removed. 274 mg {1-[4-(7-Cyano-3-phenylpyrimido[1,2-b]indazol-2-yl)-phenyl]cyclobutyl}carbamic acid tert-butylester were obtained which were used without purification in the next step (cleavage of the protecting group).

Provenance & Evidence