反应详情

温度

100 °C

A suspension of 8-chloro-imidazo[1,5-a]pyridine-7-carboxylic acid methyl ester (105 mg, 0.50 mmol), 4-cyclopropyl-2-fluoroaniline (101 mg, 0.60 mmol), Pd2dba3 (18 mg, 0.02 mmol), 2-dicyclohexylphosphino-2′,6′-diisopropoxybiphenyl (37 mg, 0.08 mmol) and K3PO4 (148 mg, 0.70 mmol) in toluene (2 mL) was degassed and then heated to 100° C. for 24 hours. The reaction mixture was then cooled to room temperature and diluted with ethyl acetate. The resultant solution was washed with water and brine, then loaded onto a 10 g Isolute® SCX-2 cartridge which was eluted with methanol followed by a 2M solution of ammonia in methanol. The appropriate fractions were combined and concentrated. The resultant residue was subjected to flash chromatography (Si-PPC, gradient 0% to 10%, ethyl acetate in dichloromethane) to afford the title compound as a yellow oil (68 mg, 42%). LCMS (method B): RT=3.45 min, [M+H]+=326.

1. customwas degassed
2. temperatureThe reaction mixture was then cooled to room temperature
3. additiondiluted with ethyl acetate
4. washThe resultant solution was washed with water and brine
5. washwas eluted with methanol
6. concentrationconcentrated