Tris(dibenzylideneacetone)dipalladium-chloroform, A common heterocyclic compound, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.”52522-40-4
A mixture of 55 mg (0.53 mmol) Pd2(dba)3CHCl3 and 200 mg(0.11 mmol) of [Mo3S4Cl3(dnbpy)3]PF6 in 20 ml of dichloromethanewas refluxed for 1 day. An excess of hexane was layeredonto the resulting brown solution to give brown crystals of 3.Yield: 113 mg (57percent). Anal. Calcd for C84H132N6Cl4Mo3S4Pd: C53.4, H 7.0, N 4.5, S 6.8. Found: C 53.6, H 7.1, N 4.4, S 6.9. 1HNMR (500.13 MHz, CDCl3): delta = 9.78 (d, J = 5.75 Hz, 3H), 9.35 (d, J= 5.62 Hz, 3H), 7.99 (s, 3H); 7.93 (s, 3H); 7.25 (d, J = 5.50, 6H),2.76 (t, J = 6.75 Hz, 6H), 2.71 (t, J = 7.7 Hz, 6H), 1.68 (p, J12 = 7.95,J23 = 7.82 Hz, 6H), 1.39 (p, J12 = 7.7, J23 = 7.1 Hz, 6H), 1.29 (s, 72H),0.89 (s, 18H) ppm. IR (KBr, cm1): 3376 (w, sh), 3223 (w), 3123(w), 2923 (s), 2852 (s), 1648 (w), 1614 (vs), 1554 (m), 1486 (m),1462 (m), 1415 (s), 1376 (w), 1338 (w), 1314 (w), 1260 (m),1188 (w), 1096 (s), 1021 (m), 913 (w), 873 (m), 802 (m),766 (w), 721 (w), 698 (w), 615 (w), 474 (w), 421 (w). ESI-MS(+; CH2Cl2/CH3CN): m/z = 1893 {H[Mo3S4(PdCl)Cl3(dnbpy)]}+,1855 [Mo3S4(Pd)Cl3(dnbpy)]+, 1348 [Mo3S4Cl3(dnbpy)]+.
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Reference£º
Article; Laricheva, Yuliya A.; Gushchin, Artem L.; Abramov, Pavel A.; Sokolov, Maxim N.; Polyhedron; vol. 154; (2018); p. 202 – 208;,
Chapter 1 An introduction to palladium catalysis
Palladium/carbon catalyst regeneration and mechanical application method