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For syntheses of supported variants of 3, 4, see inter alia: (a) Kingsbury, J. S.; Garber, S. B.; Giftos, J. M.; Gray, B. L.; Okamoto, M. M.; Farrer, R. A.; Fourkas, J. T.; Hoveyda, A. H. Angew. Chem. Int. Ed. 2001, 40, 4251.
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28844476027
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in his Diploma thesis Hannover
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Part of the work was described by K. Mennecke in his Diploma thesis (Hannover 2004).
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Mennecke, K.1
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note
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3 and finally dried under reduced pressure to yield PVP (4.85 mmol/g capacity).
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47
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85034336744
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note
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Indeed, this idea has been shown to be powerful for the immobilisation of enzymes using nickel NTA-linkers on sepharose for coordinatively trapping enzymes tagged with a His-tag.
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28844479576
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Preparation of Functionalised Poly vinyl Pyridines 6a and 6b. A suspension of ruthenium catalyst 5 (140 mg, 0.16 mmol; prepared according to ref. 16) and PVP (6a: 400 mg, 1.84 mmol; 6b: 373 mg, purchased from Acros) in toluene (3 mL) was shaken under argon at r.t. for 72 h. The polymer was filtered and washed with five portions of toluene (2 mL) to yield functionalised polymer 6 (polymer obtained by precipitation polymerisation: 510 mg, 0.15 mmol ruthenium; 96% and polymer from Acros: 477 mg, 0.09 mmol ruthenium; 80%).
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28844492998
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note
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In comparison, treatment of catalyst 5 with pyridine yielded a new material which from mass spectrometric analysis does not contain bromine but which turned out to be highly unstable and quickly degraded under nitrogen even at -20 °C.
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note
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th run (6 h; 4.8 mg, 22 μmol; 10%).
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Recently, Grubbs and coworkers were able to isolate a ruthenium-hydrido complex, formed as a thermal degradation product of catalyst 2 which could be made responsible for double-bond migration: Hong, S. H.; Day, M. W.; Grubbs, R. H. J. Am. Chem. Soc. 2004, 126, 7414.
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(b) Arisawa, M.; Terada, Y.; Nakagawa, M.; Nishida, A. Angew. Chem. 2002, 114, 4926.
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(a) Ahmed, M.; Arnauld, T.; Barrett, A. G. M.; Braddock, D. C.; Procopiou, P. A. Synlett 2000, 1007.
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note
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(b) Reaction was carried according to the general procedure given for the metathesis reactions with polymer 6a. Additionally, 1-octene (5 mol%) was added to the reaction mixture to yield 2,5-dihydro-1-tosyl-1H-pyrole(15) in 35% instead of 96% without 1-octene.
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