Poly(phenylene oxide) (PPO) - aromatic polyester multiblock copolymers were synthesized by polycondensation of bisphenol-A / isophthalic acid or m- and p-hydroxybenzoic acids in the presence of PPO having a carboxylic acid at one end and a phenolic hydroxy group at the other using triphenylphosphine / hexachloroethane as coupling agent. TG analysis showed that the multiblock copolymer showed relatively high thermal stability.