Herein, reporting a simple, sustainable, and cost-effective chemical synthesis of a star-shaped silicon-containing arylacetylene (SSA) resin via a one-pot process using zinc powder as a catalyst. The as-prepared viscous liquid resins exhibited moderate rheological behavior. The thermal curing temperature was determined to be 203 C using differential scanning calorimetry, which is much lower than that reported for polyimide and phthalonitrile (>300 C), indicating the SSA resins are suitable for processing at a lower temperature. Thermogravimetric analysis also revealed the excellent thermal stability and extremely high carbon residue of the cured SSA resin (the temperature at 5% mass loss and residual yield at 800 C under N 2 were 654 C and 93%, respectively). The results showed the excellent processability and thermal stability of SSA resin.