Improved synthesis of pincer ligand precursor, and synthesis and structural characterization of terphenyl scaffolded S-C-S palladium pincer complex

Inorganic Chemistry Communications

Volumn 12, Issue 12, 2009, Pages 1171-1174

  Schroder, Paul M ^a   Spilker, Thomas F ^a   Luu, Wilson ^a   Updegraff III, James B ^b   Kwan, Man Lung ^a   Challen, Paul R ^a   Protasiewicz, John D ^b  

^a JOHN CARROLL UNIVERSITY   (United States)

^b CASE WESTERN RESERVE UNIVERSITY   (United States)

Author keywords

Bromination; Palladium; Pincer complex; Structure; Sulfur

Indexed keywords

EID: 70449708936     PISSN: 13877003     EISSN: None     Source Type: Journal    
DOI: 10.1016/j.inoche.2009.08.036     Document Type: Article

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13. 2NEt, followed by 3 × 100 mL portions of 10% NaCl(aq). After separating the organic layer and drying with magnesium sulfate the ether and THF were removed on a rotary evaporator. The resulting oil partially crystallized after standing in the refrigerator for 2 days. Trituration of the oil and solid with ethanol led to the formation of and off-white solid which was separated from the orange ethanol solution by filtration and washed with ethanol followed by pentane. This yielded an off-white solid 2, 6.9 g (48% yield), whose NMR properties matched those as reported previously.
14. 3): δ 21.29, 38.09, 38.19, 106.68, 107.23, 127.24, 127.27, 127.70, 128.40, 129.28, 129.37, 129.82, 129.85, 129.90, 129.99, 130.26, 131.14, 131.20, 132.85, 132.95, 135.30, 135.50, 136.71, 136.84, 145.26, 145.30, 146.35, 146.44.
15. 3): δ 21.28, 40.05, 124.86, 127.72, 128.41, 128.68, 129.34, 129.88, 129.91, 131.12, 139.47, 143.60, 143.86.
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