Abstract
Diynes were synthesized in high yields by homocoupling of terminal arylacetylenes and terminal alkylacetylenes in Cu(OAc)2‐PEG (polyethyleneglycol) with NaOAc as a base. Cu(OAc)2‐PEG was readily recycled via solvent precipitation with efficient recyclability.
Acknowledgment
We thank the Natural Science Foundation of China (no. 20373061).