Abstract The synthesis of a mixture of deuterated cyclopentadiene adducts (3) required for the pyrolytic generation of CHD= C= C= O and CD 2= C= C= O is described. Methyleneketene is conveniently generated for microwave spectroscopy by flash vacuum pyrolysis of acrylic anhydride at 510-560. Pyrolysis of diphenylmethyl propiolate gives benzophenone and methyleneketene (or its decomposition products) as the major ...