反应详情

To a stirred solution of 6-amino-4-[(3-bromo-phenyl)amino]pyrido[3,2-d]pyrimidine (J Med Chem, 1996;39:1823) (46 mg, 0.15 mmol) and acrylic acid (6 mol eq., 0.91 mmol, 62 μL) in DMA (5.0 mL) under N2 was added 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDCI.HCl) (4.0 mol eq., 0.61 mmol, 116 mg). The reaction mixture was stirred for 48 hours with additional amounts of acrylic acid and EDCI.HCl (62 μL/116 mg) being added every 12 hours it was then worked up as above to give after chromatography on silica gel eluting with EtOAc:CH2Cl2 (1:1) to MeOH/CH2Cl2/EtOAc (2:48:50), N-[4-[(3-bromophenyl)-amino]pyrido[3,2 -d]pyrimidin-6-yl]acrylamide (14 mg, 26%) as a cream powder, mp (CH2Cl2/hexane) 226-228° C.

1. additionbeing added every 12 hours it