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Organometallics
Volumn 27, Issue 9, 2008, Pages 1967-1969
Synthesis and reactivity of P-chiral tethered (η1: η6-phosphinoarene)ruthenium complexes
Author keywords

[No Author keywords available]
Indexed keywords

CHEMICAL REACTIVITY; CHIRALITY; COMPLEXATION; ORGANOMETALLICS; SYNTHESIS (CHEMICAL);
EID: 44449138544     PISSN: 02767333     EISSN: None     Source Type: Journal    
DOI: 10.1021/om800076x     Document Type: Article
Times cited : (23)
References (27)
  • 15
    • 44449142479 scopus 로고    scopus 로고
    • Typical procedure for the synthesis of phosphines a-f: (S)-tert-butyl(2-phenylethyl)methylphosphine-borane (a, )-Sparteine (5.53 g, 23.6 mmol) was dissolved in 50 mL of diethyl ether, and the solution was cooled to -78°C with stirring. A sec-butyllithium solution (17.5 mL of 1.3 M solution in hexanes) was added by syringe. After 10 min, a solution of tert-butyldimethylphosphine-borane (2.50 g, 18.9 mmol) in diethyl ether (45 mL) was added by syringe and the solution was stirred at -78°C. Three hours later benzyl bromide (3.40 mL, 28.3 mmol) was added. The reaction mixture was warmed to room temperature overnight and then was quenched by the addition of 50 mL of water. The suspension was extracted with diethyl ether (3 × 40 mL, The combined organic layers were dried with sodium sulfate and filtered, and the solvent was removed in vacuo. The resulting residue was purified by chromatography on silica gel hexane-ethyl acetate, increasing polarity, furnishing the product
    • 13C NMR, IR, and elemental analysis data are given in the Supporting Information.
  • 16
    • 44449171422 scopus 로고    scopus 로고
    • Typical procedure for the synthesis of complexes 2: dichloro(η 6-p-cymene, R)-tert-butylmethyl(2-phenylethyl)phosphine) ruthenium(II)(2a, A 2.00 mL portion of tetrafluoroboric acid diethyl ether complex (2.38 g, 14.6 mmol) was slowly added to a stirred, cooled (0°C) solution of 0.80 g (3.6 mmol) of a in 18 mL of CH2Cl2. After 1 h, the ice bath was removed and conversion was monitored by 31P{1H} NMR. To the reaction mixture were added 30 mL of CH2Cl2 and 80 mL of degassed, aqueous saturated NaHCO 3 solution. The organic layer was separated, and the aqueous layer was extracted with CH2Cl2 (3 × 20 mL, The was reduced to 20 mL, and 0.60 g of [Ru(μ-Cl)Cl(η6-p-cymene, 2 (0.99 mmol) was added. After 30 min the conversion was monitored by 31P{1H} NMR and the rest of the [Ru(μ-Cl) Clη6-p-cymen
    • 13C NMR, IR, and elemental analysis data are given in the Supporting Information.
  • 18
    • 44449134221 scopus 로고    scopus 로고
    • -1; λ = 0.710 73 Å; T= 293 K; 17 326 reflections collected (R(int) = 0.0390); final R indices (I > 2σ(I)) R1 = 0.0316, wR2 = 0.0864, GOF = 1.178. CCDC 652572 contains the supplementary crystallographic data for this structure. These data can be obtained free of charge from The Cambridge Crystallographic Data Centre via www.ccdc.cam.ac.uk/data_request/cif.
    • -1; λ = 0.710 73 Å; T= 293 K; 17 326 reflections collected (R(int) = 0.0390); final R indices (I > 2σ(I)) R1 = 0.0316, wR2 = 0.0864, GOF = 1.178. CCDC 652572 contains the supplementary crystallographic data for this structure. These data can be obtained free of charge from The Cambridge Crystallographic Data Centre via www.ccdc.cam.ac.uk/data_request/cif.
  • 27
    • 33847188871 scopus 로고    scopus 로고
    • Recent mechanistic studies: Chaplin, A. B.; Fellay, C.; Laurenczy, G.; Dyson, P. J. Organometallics 2007, 26, 586.
    • Recent mechanistic studies: Chaplin, A. B.; Fellay, C.; Laurenczy, G.; Dyson, P. J. Organometallics 2007, 26, 586.

* 이 정보는 Elsevier사의 SCOPUS DB에서 KISTI가 분석하여 추출한 것입니다.