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- Title
Preparation of Thiophene-Fused and Tetrahydroquinoline-Linked Cyclopentadienyl Titanium Complexes for Ethylene/α-Olefin Copolymerization.
- Authors
Sung Hun Kim; Ji Hae Park; Bo Geun Song; Seung-Woong Yoon; Min Jeong Go; Junseong Lee; Bun Yeoul Lee
- Abstract
A synthetic scheme was developed for the large-scale preparation of a dimethylthiophene-fused and tetrahydroquinaldine-linked dimethylcyclopentadienyl titanium complex (2), which is a high-performance homogeneous Ziegler catalyst. 2,3,4,5-Tetramethyl- 4,5-dihydrocyclopenta[b]thiophen-6-one was prepared without chromatography purification on the 40-g scale in a laboratory setting, from which the ligand precursor for 2 was obtained in 65% yield on a 50-g scale in a one-pot without the need for chromatography purification. Metallation was achieved in a high yield (78%) through reaction of the dilithiated compound with TiCl4. Many derivatives were prepared by employing the same synthetic scheme as applied for 2. Among them, the titanium complex prepared from 2-methyl-4,5-dimethyl-6-(2-n-butyl-2,3,4,5-tetrahydroquinolin-8-yl)-4H-cyclopenta[b]thiophene exhibited an exceptionally high activity. Under commercially relevant high-temperature polymerization conditions (160 °C), this compound showed a higher activity than 2 (126 x 106 g/molTi*h versus 72 x 106 g/molTi*h), albeit with the formation of a polymer of slightly lower molecular weight (Mw, 159,000 versus 218,000) and with a slightly lower 1-octene content (9.3 mol% versus 12 mol%).
- Subjects
TITANIUM compounds; METALLOCENES; THIOPHENES; CYCLOPENTADIENE; POLYMERIZATION research; MOLECULAR weights
- Publication
Catalysts (2073-4344), 2013, Vol 3, Issue 1, p104
- ISSN
2073-4344
- Publication type
Article
- DOI
10.3390/catal3010104