A new method was developed using ultrasonic irradiation to synthesize poly(2-methoxy-5-butoxy) phenylene vinylene from p-methoxy phenol (MOPh) and CH3 (CH2)3Br. Ultrasonic irradiation catalyzes the reactions through three major steps of etherification, bischloromethylation and elimination. Results showed that our ultrasonic irradiation method could significantly enhance production yield and reduce process time of the synthesis compared with reflux agitating method.