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Volumn 9, Issue 10, 2007, Pages 1955-1957

Efficient removal of ruthenium byproducts from olefin metathesis products by simple aqueous extraction

Author keywords

[No Author keywords available]

Indexed keywords

ALKENE; DIETHYL DIALLYLMALONATE; MALONIC ACID DERIVATIVE; RUTHENIUM DERIVATIVE; UNCLASSIFIED DRUG;

EID: 34249281622     PISSN: 15237060     EISSN: None     Source Type: Journal    
DOI: 10.1021/ol070512j     Document Type: Article
Times cited : (76)

References (24)
  • 2
    • 1442360753 scopus 로고    scopus 로고
    • Grubbs, R. H, Ed, Wiley-VCH: Weinheim, Germany, Vols
    • Handbook of Metathesis; Grubbs, R. H., Ed.; Wiley-VCH: Weinheim, Germany, 2003; Vols. 1-3.
    • (2003) Handbook of Metathesis , vol.1-3
  • 22
    • 34249338774 scopus 로고    scopus 로고
    • A typical purification procedure is as follows: Crude 3,3-diethylester-pentene (6, 100 mg, 0.472 mmol) in diethyl ether (∼30 mL) was transferred to a separatory funnel. The diethyl ether solution was washed three or five times by water (∼30 mL, dried over MgSO 4, and concentrated. Approximately 20∼30 mg of the resulting clear oil was accurately weighed by a microbalance and digested with concentrated nitric acid overnight for ICP-MS analysis. For activated carbon purification, the activated carbon (1.3 wt equiv of the crude product 6) was added to the diethyl ether solution after the extraction and stirred for 24 h. After the carbon was filtered, the filtrate was concentrated in vacuo to provide 6 as clear oil. THMP and DMSO methods were carried out following the literature procedures except avoiding silica gel treatment or column chromatography
    • 4, and concentrated. Approximately 20∼30 mg of the resulting clear oil was accurately weighed by a microbalance and digested with concentrated nitric acid overnight for ICP-MS analysis. For activated carbon purification, the activated carbon (1.3 wt equiv of the crude product 6) was added to the diethyl ether solution after the extraction and stirred for 24 h. After the carbon was filtered, the filtrate was concentrated in vacuo to provide 6 as clear oil. THMP and DMSO methods were carried out following the literature procedures except avoiding silica gel treatment or column chromatography.


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