Falling‐Solid Flash Vacuum Pyrolysis: An Efficient Preparation of Arylacetylenes

Automated falling-solid flash vacuum pyrolysis allows the rapid and efficient synthesis of a variety of arylacetylenes from 4-arylmethylidene-5(4H)-isoxazolone derivatives, which were prepared from aldehyde precursors. The acetylenes are readily obtained in multigram quantities.