Water-soluble metal-based complex and preparation method and application thereof
A metal-based and complex technology, applied in the preparation of carbon-based compounds, organic compounds, carbon monoxide reaction preparation, etc., can solve the problems of difficult hydroformylation and low water solubility
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[0061] As the preparation method of the above-mentioned water-soluble metal-based complex, the synthetic method of the rhodium-based complex is as follows:
[0062]
[0063] The soluble metal-based complex is obtained through a coordination reaction between a rhodium precursor RhY and a sulfonate-type bisphosphine ligand in a solvent under CO flow. Specifically, the coordination reaction temperature is 0-100°C. Preferably, the coordination reaction time is 0.5-48h. The solvent can be one or both of alcohols and water. Preferably, the alcohols are methanol and / or ethanol.
[0064] This class of novel water-soluble rhodium-based complexes in this application has the following unique advantages: (1) Compared with conventional rhodium precursors such as Rh(acac)(CO) 2 , the solubility of the water-soluble rhodium-based complex increases in water, and the coordination of the sulfonate-type bisphosphine ligand improves the stability of the catalyst, which can reduce the loss o...
Embodiment 1
[0078] Water-soluble rhodium-based complex 1 (-5-Cl) (representing 1 coordinated by 5 and Cl), its structural formula is as follows:
[0079]
[0080] The specific preparation method is as follows: add 1.0 mmol of RhCl to a 50 mL Schlenk bottle in the glove box 3 ·H 2 O and sulfonate type bisphosphine ligand 5 1.0mmol and 20mL ethanol, the reaction mixture was taken out from the glove box, and carbon monoxide gas (purity 99.99%) was introduced at a flow rate of 15mL / min, and the temperature was raised to 40°C, and reaction 3 Hour. Then cooled to room temperature and filtered, the obtained yellow precipitate was washed with ethanol until neutral, and then dried under vacuum at 60 °C overnight to obtain a light yellow solid with a yield of 90% based on Rh.
[0081] of the final prepared product 1 H NMR (CD 3 CD): δ7.79-7.15(m,24H,ArH)
Embodiment 2
[0083] Water-soluble rhodium-based complex 1 (-5-acac) (representing 1 coordinated by 5 and acac), its structural formula is as follows:
[0084]
[0085] Its specific preparation method is: add 1.0mmol Rh(acac)(CO) in the 50mL Schlenk bottle in the glove box 2 and sulfonate-type bisphosphine ligand 5 1.0mmol and 20mL ethanol, the reaction mixture was taken out from the glove box, and carbon monoxide gas (purity 99.99%) was introduced at a flow rate of 15mL / min, and the temperature was raised to 40°C, and the reaction was carried out for 3 hours . Then cooled to room temperature and filtered, the obtained yellow precipitate was washed with ethanol until neutral, and then dried in vacuum at 60 °C overnight to obtain a pale yellow solid with a yield of 95% based on rhodium.
[0086] 1 H NMR (CD 3 CD): δ7.69-7.11(m,24H,ArH),3.61(s,2H,CH 2 ),2.25(s,6H,CH 3 ).
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