AbstractWe developed an environmentally benign, convenient microwave‐assisted process for the construction of 1,3,5‐trisubstitued pyrazolines (10a∼10f, 11a∼11f, 12a∼12f, 13a∼13f). Chalcones, as the key intermedi‐ ates, were obtained by the condensation of each of appropriately substituted aromatic aldehydes (1∼4) with 4‐substituted acetophenones (5a∼5f) via a Claisen‐Schmidt reaction under the action of microwave irradiation. Cyclization of the chalcones (6a∼6f, 7a∼7f, 8a∼8f, 9a∼9f) with p‐toluene sulfonhydrazide af‐ forded 1,3,5‐trisubstitued pyrazoline derivatives using microwave‐assisted process in 25 min and 140 watt power in glycol. The structures of targeted compounds were established by IR, 1H NMR, MS and ele‐ mental analysis. The results indicate that microwave‐assisted synthetic process presents advantages in terms of enhancement in rate, decrease in reaction time, clean reaction and convenient operation.