Unsymmetrical salts, ccc-nhc pincer metal complexes, and methods of making the same
A CCC-NHC, metal complex technology, applied in the direction of organic compounds/hydrides/coordination complex catalysts, iron organic compounds, platinum organic compounds, etc.
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Embodiment 1
[0105] Synthesis and anion exchange of azoles and salts
[0106] Monoheterocyclic azole—oxazole (21.2mmol), 1,3-dibromobenzene (5.00g, 21.2mmol), CuO (506mg, 6.36mmol), K 2 CO 3 (4.40 g, 31.8 mmol) and 75 mL DMSO were mixed and heated at 150° C. for 48 hours. The reaction was cooled, a mixture of dichloromethane and isopropanol (150 mL, ratio = 10:1) was added and it was filtered through a pad of basic alumina. The alumina pad was washed with dichloromethane and isopropanol mixture (500 mL, ratio=10:1), and the resulting filtrate was concentrated under reduced pressure to obtain a solid, which was purified by silica gel column chromatography.
[0107] Monoazolium Salt - 1-(3-Bromophenyl)azole (2.77mmol), alkyl halide (55.4mmol) and acetonitrile (5.71g) were mixed and stirred at 120°C. After cooling to room temperature, the volatiles were removed under reduced pressure to give a white solid.
[0108] Unsymmetrical bis(azole)—bromoarylazole (22.5mmol), heterocyclic azole (22...
Embodiment 2
[0123] Synthesis and Characterization
[0124] Ligands 1, 2 and 3 were synthesized using the adapted method. Ligands 4, 5 and 6 and iodonium salts 9 and 10 were synthesized according to published procedures. Using a similar alkylation procedure, the chloride salts 7 and 8 were synthesized from butyl chloride and neohexyl chloride, respectively, as Figure 8 shown. Tetraphenylborates (11, 12) were synthesized in high yields (81% and 99%, respectively) by reacting the corresponding iodide salts with sodium tetraphenylborate in methanolic solution (see Figure 8 ).
[0125] like Figure 9 As shown, an asymmetric CCC-NHC pincer platinum complex was synthesized for the first time. Synthesis of complexes 13-16 was performed following standard procedures. like Figure 10 As shown, the platinum-bound chloride of complex 13 was replaced by OAr groups.
[0126] Monocoordinate metal complexes
[0127] The monodentate metal complexes of formula III can generally be described as a...
Embodiment 3
[0162] Bicoordinate metal complexes
[0163] Bicoordinate metal complexes of formula IV can generally be described by alternative forms of formula VII.
[0164]
[0165] M = any transition metal, metal or metalloid (especially Rh, Ir, Co, Ni, Pd, Pt, Fe, Ru, Os, Mn, V, Cu).
[0166] E. 1 ,E 2 = C or N, E 1 can be equal to E 2 , or E 1 May not be equal to E 2 , n represents the charge on the complex and it can be negative or positive, usually in the range of -2 to +3, but may not be within this range.
[0167] n' represents the number of counterions (X) required to balance the charge n on the pincer complex.
[0168] R 1 , R 2 , R 3 , R 4 = is an alkyl or aryl substituent containing 1-50 carbons and may contain heteroatoms such as N, O and S. These substituents may be all the same, all may be different, or any combination of the two.
[0169] het 1 、het 2 、het 3 and het 4 is defined as a nitrogen-based heterocyclic ring containing one or more nitrogen atoms an...
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