A series of phenyl, substituted phenyl and thiophene bearing dihydrofuropyrimidin‐4‐ones (3a‐p) were synthesized by Mn(OAc)3 mediated, microwave irradiated radical cyclizations of 2‐hydroxy‐pyridopyrimidin‐4‐one derivatives (1a‐j) with substituted phenylvinylthiophenes (2a‐c) at 70°C in 2 min. Compounds 3a‐j was obtained between 28% and 66% yields. Molecular structures of 3a‐p were determined by 1H NMR, 13C NMR, 19F NMR, FTIR and HRMS techniques. Inhibitory activity of 3a‐p were evaluated against Acetylcholinesterase (AChE) and inhibition results of these compounds showed that the compounds had good inhibition with IC50 values between 0.52 and 3.77 μM. In addition, molecular docking studies were carried out on the most potent inhibitory compounds 3d (IC50 = 0.64 μM), 3p (IC50 = 0.52 μM) and standart drug Donepezil. The binding energies for 3d, 3p and Donepezil are −9.12, −10.08 and −12.65 Kcal/mol, respectively. Based on these results, it was determined that, compounds 3d and 3p are promising AChE inhibitors.