Abstract

Abstract1H‐NMR spectra of polyisoprene were assigned using polymers of isoprene‐1,1,4,4‐d4, isoprene‐1,1,5,5,5‐d5, and isoprene‐4,4‐d2 polymerized with various catalysts. The methylene‐proton signal at 2.1 ppm in cis‐1,4 ‐ and trans‐1,4‐polyisoprenes was divided into H4‐ and H1‐proton signals; H4 resonated at 2.21 ppm in both cis‐1,4 and trans‐1,4 units whereas H1 resonated at 2.05, 2.21, and 2.15 ppm. Splitting due to the dyad sequences of 1,4 and 3,4 units was apparent. The methine‐proton (H3) in a 3,4 unit showed a broad peak centered around 1.5 ppm in C6D6. The overlapping of this signal with the methyl‐proton signals at 1.73 and 1.63 ppm resulted in some uncertainty in the determination of the microstructure of polyisoprene which contained a considerable amount of 3,4 unit.

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