反应详情

温度

100 °C

A suspension of 8-chloro-imidazo[1,5-a]pyridine-7-carboxylic acid methyl ester (223 mg, 1.06 mmol), 2-fluoro-4-methylsulfanyl-phenylamine (200 mg, 1.27 mmol), Pd2dba3 (39 mg, 0.04 mmol), 2-dicyclohexylphosphino-2′,6′-diisopropoxybiphenyl (79 mg, 0.17 mmol) and K3PO4 (315 mg, 1.48 mmol) in toluene (4 mL) was degassed and then heated at 100° C. for 18 hours. The reaction mixture was then cooled to room temperature and diluted with ethyl acetate. The resultant mixture was washed with water followed by brine, before being loaded onto a 10 g Isolute® SCX-2 cartridge which was eluted with methanol, and then a 2M solution of ammonia in methanol. The appropriate fractions were combined and concentrated in vacuo to give a residue. The residue was subjected to flash chromatography (Si-PPC, gradient 0% to 10%, ethyl actetate in dichloromethane) to afford the title compound as a yellow oil (136 mg, 39%). LCMS (method B): RT=3.26 min, [M+H]+=332.

1. customwas degassed
2. temperatureThe reaction mixture was then cooled to room temperature
3. additiondiluted with ethyl acetate
4. washThe resultant mixture was washed with water
5. washwas eluted with methanol
6. concentrationconcentrated in vacuo
7. customto give a residue