Phosphoramidite carbonyl rhodium hydride catalyst as well as preparation method and application thereof
A carbonyl hydrogenation rhodium, phosphoramidite technology, applied in the preparation of carbon-based compounds, carbon monoxide reaction preparation, physical/chemical process catalysts, etc., can solve problems such as low efficiency and poor effect
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Embodiment 1
[0031] This embodiment provides a kind of preparation method of phosphoramidite carbonyl rhodium hydride catalyst, comprising the following steps:
[0032] The phosphine ligand binaphthol bisindolyl phosphine L1 and the metal rhodium precursor Rh(acac)(CO) 2 Put into the autoclave with a molar ratio of 1:1, add toluene solvent, replace with synthesis gas, fill with 1MPa synthesis gas and stir at room temperature for 2 hours, take out the reaction liquid and remove the solvent to obtain a yellow solid The target product HRh(L1)(CO) 2 , the product was subjected to nuclear magnetic resonance (NMR) P spectrum ( 31 P NMR) and H spectrum ( 1 H NMR) test, the result is as figure 1 and figure 2 as shown, 31 P signal in P NMR is 137.09, J Rh-P is 217.08, 1 The characteristic negative hydrogen signal in H NMR is -10.39.
Embodiment 2
[0034] This embodiment provides a kind of preparation method of phosphoramidite carbonyl rhodium hydride catalyst, comprising the following steps:
[0035] The phosphine ligand biphenol bis(6-methoxy)-indolylphosphine L2 and the metal rhodium precursor Rh(acac)(CO) 2 Put into the autoclave with a molar ratio of 1:1, add toluene solvent, replace with synthesis gas, fill with 2MPa synthesis gas and stir at room temperature for 2 hours, take out the reaction liquid and remove the solvent to obtain a yellow solid The target product HRh(L2)(CO) 2 , the product was subjected to nuclear magnetic resonance (NMR) P spectrum ( 31 P NMR) and H spectrum ( 1 H NMR) test, the result is as image 3 and Figure 4 as shown, 31 P signals in P NMR are 136.74, 135.40, J Rh-P is 217.08, 1 The characteristic negative hydrogen signal in H NMR is -10.85.
Embodiment 3
[0037] This embodiment provides an application example of the catalyst of the present invention in olefin hydroformylation reaction, the operation is as follows:
[0038] With the catalyst prepared by embodiment 1---phosphoramidite carbonyl rhodium hydride [HRh (L1) (CO) 2 ] 0.02mmol, wherein L1 is phosphoramidite ligand, adds autoclave, and according to the amount of substance alkene: the ratio that catalyst is 1000 adds 1-hexene and carries out hydroformylation, reacts under 80 ℃, 10bar synthesis gas After 2 hours, analyze the product content by gas chromatography, the results are as follows:
[0039]
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