X-Ray structure of a novel product formed from 2,5-dimethylhex-3-yne-2,5-diol by catalytic action of dibromobis(triphenylphosphine)nickel
- 1 January 1977
- journal article
- research article
- Published by Royal Society of Chemistry (RSC) in Journal of the Chemical Society, Perkin Transactions 2
- No. 8,p. 1011-1015
- https://doi.org/10.1039/p29770001011
Abstract
When heated under reflux in toluene in the presence of [(Bun 3P)2NiBr2], 2,5-dimethylhex-3-yne-2,5-diol is not converted into the expected simple polymerization product. X-Ray structural analysis shows the novel product to be 1′-(1,3-dihydro-7-isopropenyl-6-isopropyl-1,1,4,4-tetramethylfuro[3,4-c]pyran-3-ylidenemethyl)-1,3-dihydro-7-isopropenyl-6-isopropyl-1,1,4,4,5′,5′-hexamethylfuro[3,4-c]pyran-3-spiro-3′-cyclohexene, in agreement with other physical data. The same product was obtained with [(Ph3P)2NiBr2] as catalyst. Crystals are monoclinic, a= 9.32(1), b= 37.26(3), c= 13.18(1)Å, β= 118.7(1)°, Z= 4, space group P21/c. The structure was solved from diffractometer data by direct methods and refined to R 0.054 for 3 583 observed reflections.Keywords
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