80% |
In methanol; dichloromethane; at 20.0℃; for 24.0h;Inert atmosphere; Darkness; Reflux; |
1,1'-Bis(di-tert-butylphosphino) ferrocene (dtbpf) (0.474 g, 1.0 mmol) was added to a solution of silver(I) cyanide (0.134 g, 1.0 mmol) in 30 mL CH3OH:CH2Cl2 (50:50 V/V) mixture in dark atroom temperature. The resultant suspension was refluxed with stirring under nitrogen atmosphere for 24 h. Slowly, the colour ofthe solution changed from light orange to dark yellowish red colour. The resulting solution was evaporated to dryness to give a yellowish red solid which was then extracted with dichloromethane (20 mL). The addition of hexane (100 mL) to this solution led to yellowish red rod shaped diffraction quality crystals. These were separated and washed with hexane and dried. Yield: (0.808 g, 80 %). Anal. Calc. for C30H44N4P2Ag4Fe: C, 35.64;H, 4.36; N, 5.54. Found: C, 35.82; H, 4.40; N, 5.64. IR (cm-1, KBr): nu = 3410, 3095, 2987, 2947, 2899, 2867, 2718, 2459, 2114(CN), 1645, 1477, 1458, 1392, 1368, 1302, 1216, 1175, 1154, 1040, 1021, 932, 887, 812, 751, 663, 630. 1H NMR ( delta ppm, 400 MHz, CDCl3, 298 K), 4.35 (s, 4H, C5H4), 4.15 (s, 4H, C5H4),1.21 (m, 36H, CH3). 31P{1H}: delta 41.54 (sbr). UV/Vis: lambdamax (epsilon [dm3 mol-1 cm-1]) 265 (20,432), 474 (18,890). ESI-MS (m/z): 1009.4 (M+). |