Mixed nickel (II) complex based on phosphite and unsaturated n-heterocyclic carbene as well as preparation method and application thereof
A nitrogen-heterocyclic carbene and phosphite technology, which is applied in the field of nickel complexes and their organic synthesis, can solve the problems of no hydrogenation addition reaction, etc., and achieve the effect of improving operability, low toxicity, and facilitating coordination
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[0028] Example 1: Ni[P(OR 1 ) 3 ][(R 2 NCHCHNR 2 )C]X 2 (R 1 =ethyl, R 2 =2,4,6-trimethylphenyl, X=bromo) synthesis
[0029] The unsaturated nitrogen heterocyclic carbene (R 2 NCHCHNR 2 ) C (0.3042g, 1.0 mmol) was added to a tetrahydrofuran solution of bis(triethyl phosphite) nickel(II) dibromide (0.5500 g, 1.0 mmol), reacted at room temperature for 2 hours, and the solvent was removed in vacuo. The residue was washed with n-hexane, the obtained residue was extracted with toluene, the clear liquid was transferred and the solvent toluene was removed to obtain a red solid with a yield of 68%.
[0030] Elemental analysis of the product, the results are shown in Table 1:
[0031] Table 1 Elemental analysis results
[0032] C: (%) H: (%) N: (%) Theoretical value46.995.844.06 Actual value 47.165.934.01
[0033] The product was characterized by NMR, and the results are as follows:
[0034] Dissolve the product in C 6 D 6 Medium (about 0.4 mL), seal the tube, and measure and characterize...
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[0035] Example 2: Ni[P(OR 1 ) 3 ][(R 2 NCHCHNR 2 )C]X 2 (R 1 =isopropyl, R 2 = 2,4,6-trimethylphenyl, X=bromo) synthesis
[0036] The unsaturated nitrogen heterocyclic carbene (R 2 NCHCHNR 2 )C (0.3042g, 1.0 mmol) was added to the tetrahydrofuran solution of bis(triisopropyl phosphite) nickel(II) dibromide (0.6350 g, 1.0 mmol), reacted at room temperature for 3 hours, and the solvent was removed in vacuo , Wash the residue with n-hexane, extract the obtained residue with toluene, transfer the clear liquid and remove the solvent toluene to obtain a red solid with a yield of 72%.
[0037] The elemental analysis of the product, the results are shown in Table 2:
[0038] Table 2 Elemental analysis results
[0039] C: (%) H: (%) N: (%) Theoretical value49.216.333.83 Actual value 49.436.393.72
[0040] The product was characterized by NMR, and the results are as follows:
[0041] Dissolve the product in C 6 D 6 Medium (about 0.4 mL), seal the tube, and measure and characterize on the U...
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[0042] Example 3: Ni[P(OR 1 ) 3 ][(R 2 NCHCHNR 2 )C]X 2 (R 1 =ethyl, R 2 =2,6-Diisopropylphenyl, X=bromo) synthesis
[0043] The unsaturated nitrogen heterocyclic carbene (R 2 NCHCHNR 2 ) C (0.3883g, 1.0 mmol) was added to a tetrahydrofuran solution of bis(triethyl phosphite) nickel(II) dibromide (0.5500 g, 1.0 mmol), reacted at room temperature for 1 hour, and the solvent was removed in vacuo, The residue was washed with n-hexane, the obtained residue was extracted with toluene, the clear liquid was transferred and the solvent toluene was removed to obtain a red solid with a yield of 73%.
[0044] Elemental analysis of the product, the results are shown in Table 3:
[0045] Table 3 Elemental analysis results
[0046] C: (%) H: (%) N: (%) Theoretical value51.196.773.62 Actual value 51.316.803.57
[0047] The product was characterized by NMR, and the results are as follows:
[0048] Dissolve the product in C 6 D 6 Medium (about 0.4 mL), seal the tube, and measure and characterize ...
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