Ethynylarsine (2a) is synthesized by reaction of arsenic trichloride with ethynyltributylstannane followed by a chemoselective reduction of the formed ethynyldichloroarsine (la). The base-induced rearrangement of compound 2a on a solid base in VGSR conditions leads to ethylidynearsine (3a) characterized by 1 H and 13C NMR and by microwave spectroscopy. The rotational spectrum of 3a is recorded in the frequency range 90-470 GHz. Rotational and centrifugal distortion constants are determined and the quadrupole hyperfine structure is analyzed. The structure of CH~CIAS has been estimated from the rotational constants of eight different isotopic species and from ab initio calculations. Compound 3a exhibits a low stability at 0 OC in deuteriochloroform (~1 1 2 ca. 1 h) or in the gaseous phase at a pressure of 10 Pa (~1 / 2 ca. 30 min).
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