Abstract
Molybdenum olefin complexes of the type [Mo(NPh)(η2-olefin)(o-(Me3SiN)2C6H4)] (olefin = propene (1a), isobutene (1b)) reacted with butadiene gas, affording [Mo(NPh)(η4-H2CCHCHCH2)(o-(Me3SiN)2C6H4)] (2), a molybdenum η4-butadiene complex. The crystal structure of 2 is reported. Treatment of 2 with 1 equiv of 2-butyne afforded (3) by 1H NMR spectroscopy. Two intermediates arising during the progress of the reaction were trapped at low temperature and characterized as the isomeric η3-allyl metallacycles [syn-Mo(NPh)(C(CH3)C(CH3)CH2CHCHCH2)(o-(Me3SiN)2C6H4)] and [anti-Mo(NPh)(C(CH3)C(CH3)CH2CHCHCH2)(o-(Me3SiN)2C6H4)] (4a,b, respectively) by NMR spectroscopy. Complex 3 was made independently by reaction of 1b with 1,2-dimethyl-1,4-cyclohexadiene, and the crystal structure of 3 is reported. Treatment of 2 with 2 equiv of 2-butyne afforded 1,2-dimethyl-1,4-cyclohexadiene as an organic product with concomitant formation of [Mo(NPh)(η2-alkyne)(o-(Me3SiN)2C6H4)] (alkyne = 2-butyne; 5) by 1H NMR spectroscopy. Reaction of 1b with 2-butyne also affords 5, and the X-ray structure of 5 is reported.
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