A common heterocyclic compound, the catalyst-palladium compound, name is Tris(dibenzylideneacetone)dipalladium-chloroform,cas is 52522-40-4, mainly used in chemical industry, its synthesis route is as follows.
0.1624 g (0.4076 mmol) of 1,2-bis(diphenylphosphine)ethane, 0.1671 g (1.159 mmol) of dmfu and 0.2002 g (0.1934 mmol) of [Pd2(DBA)3*CHCl3] were dissolved under inert atmosphere (Ar) in 30 ml of anhydrous acetone and vigorously stirred for 60 min. Owing to the progressive dissolution of [Pd2(DBA)3*CHCl3], the violet color of the mixture gradually disappeared and the concomitant precipitation of the scarcely soluble pale yellow complex 1j was observed. The solution was dried under vacuum, the residue dissolved in CH2Cl2, treated with activated charcoal and filtered on a celite filter. The clear pale yellow solution was concentrated under vacuum and the title complex precipitated by slow addition of diethylether. Complex 1j was filtered off on a gooch, washed with diethylether and dried under vacuum. 0.2027 g (yield 81percent) of the title complex 1j as a pale yellow solid was obtained. 1H NMR (300 MHz, CDCl3, T = 298 K, ppm) delta: 2.11-2.61 (m, 4H, CH2P), 3.40 (s, 3H, OCH3), 4.33-4.42 (m, 2H, CH=CH), 7.32-7.53 (m, 16H, PPh), 7.79-7.85 (m, 4H, PPh). 13C{1H} NMR (CDCl3, T = 298 K, ppm selected peaks) delta: 26.7 (m CH2, CH2P), 50.5 (CH3, OCH3), 52.9 (m, CH, CH=CH), 173.7 (C, CO). 31P{1H} NMR (CD2Cl2, T = 298 K, ppm) delta: 39.0. IR (KBr, pellet, cm-1): 1683 (nCO). Anal. Calcd. for C32H32O4P2Pd: C 59.22, H 4.97. Found: C 59.11, H 5.03.
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Reference£º
Article; Canovese, Luciano; Scattolin, Thomas; Visentin, Fabiano; Santo, Claudio; Journal of Organometallic Chemistry; vol. 834; (2017); p. 10 – 21;,
Chapter 1 An introduction to palladium catalysis
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