A convenient method for the efficient removal of ruthenium byproducts generated during olefin metathesis reactions

Organic Letters

Volumn 3, Issue 9, 2001, Pages 1411-1413

  Ahn, Yu Mi ^a   Yang, KyoungLang ^a   Georg, Gunda I ^a  

^a UNIVERSITY OF KANSAS   (United States)

Author keywords

[No Author keywords available]

Indexed keywords

ALKENE; DIETHYL DIALLYLMALONATE; DIMETHYL SULFOXIDE; MALONIC ACID DERIVATIVE; ORGANOPHOSPHORUS COMPOUND; RUTHENIUM; TRIPHENYLPHOSPHINE OXIDE;

ARTICLE; CATALYSIS; CHEMICAL STRUCTURE; CHEMISTRY;

ALKENES; CATALYSIS; DIMETHYL SULFOXIDE; MALONATES; MOLECULAR STRUCTURE; ORGANOPHOSPHORUS COMPOUNDS; RUTHENIUM;

EID: 0035799891     PISSN: 15237060     EISSN: None     Source Type: Journal    
DOI: 10.1021/ol010045k     Document Type: Article

References (16)

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12. 3P=O (350 mg, 50 equiv, relative to catalyst 1) or DMSO (90 μL, 50 equiv, relative to catalyst 1) overnight. The solution was concentrated in vacuo and purified by column chromatography on silica gel (2 g/0.01 mmol of catalyst 1) using hexanes: EtOAc = 8:1 as the eluent to provide the RCM product 5 in 95-98% yield.
13. Samples (approximately 5-10 mg) were accurately weighed, digested with distilled 6 N nitric acid overnight, and diluted to a total volume of approximately 100 mL with the distilled acid and distilled deionized water to a final acid concentration of about 2%. Samples were analyzed on a PQII+XS inductively coupled plasma mass spectrometer (ICP-MS). Masses 96, 98, 99, 100, 101, 102, and 104 were monitored in all samples and standards. Drift (corrected according to the method by Cheatham, M. M.; Sangrey, W. F.; White, W. M. Spectrochim. Acta, Part B 1993, 48B, E487-E506) was usually less than 5% and always less than 10% during a single run. The reported concentration is the average of the total Ru concentration as calculated from each of the individual isotopes after drift correction. The average usually had a percent relative standard deviation (%RSD) of less than 2% and always less than 4%.
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16. Dougherty, J. M.; Probst, D. A.; Robinson, R. E.; Moore, J. D.; Klein, T. A.; Snelgrove, K. A.; Hanson, P. R. Tetrahedron 2000, 56, 9781-9790.