Alkene double decomposition catalyst and preparation method thereof
A metathesis catalyst, olefin technology, applied in chemical instruments and methods, preparation of organic compounds, catalysts for physical/chemical processes, etc., can solve problems such as high cost and difficult preparation, and achieve the effects of simple synthesis and easy availability of raw materials
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[0030] In the preparation method of the catalyst of the present invention, the reaction in step (1) can be carried out in the presence of an organic solvent. The organic solvent used may be alcohol, ether or a mixture thereof, such as methanol, ethanol, propanol, butanol, ether, tetrahydrofuran, etc. or a mixture thereof; preferably methanol, ethanol or a mixture thereof. The amount of solvent used is sufficient to ensure that the reactants are fully dissolved or dispersed.
[0031] The reaction of step (1) can be carried out in the presence or absence of a catalyst. Possible catalysts are acid compounds, such as acetic acid, p-toluenesulfonic acid, etc.; strong water absorption catalysts such as molecular sieves, titanium tetrachloride, etc. can also be used.
[0032] In step (1), the molar ratio of compound (a) to hydrazine hydrate is preferably 1:0.5-1:10, more preferably 1:1-1:5, most preferably 1:1-1:3.
[0033] The reaction in step (1) can be carried out at 10-30°C, pr...
Embodiment 1
[0044] A: Catalyst C 1 preparation of
[0045] Add benzaldehyde (1.06 g, 10 mmol) and hydrazine hydrate (1.0 g, 20 mmol) into a 100 mL round bottom flask, add 20 mL of ethanol, and stir at room temperature for 1 hour. The reaction solution was extracted with n-pentane, and the extracted organic phase was dried with anhydrous magnesium sulfate, and the solvent was removed by rotary evaporation to obtain an oil-diazo compound (0.8 g, 6.8 mmol, yield 68%).
[0046] The above oily diazo compound (0.24g, 2mmol) was dissolved in 5mL of n-pentane, cooled in an ice bath, and then added into 10mL of dichloromethane dissolved in tris(triphenylphosphine)ruthenium dichloride (0.95g, 1mmol) , the mixture was cooled to -78°C and stirred for 0.5 hour. The solvent was removed by rotary evaporation, and the residue was recrystallized with dichloromethane / n-pentane (volume ratio 1:1) to obtain catalyst C 1 (0.8 g, 0.96 mmol, 96% yield).
[0047] The elemental analysis data of the product is...
Embodiment 2
[0051] Example 2 Catalyst C 2 preparation of
[0052] The preparation method is the same as in Example 1, but benzaldehyde is replaced by o-chlorobenzaldehyde to obtain catalyst C 2 , whose elemental analysis data is C 43 h 35 Cl 3 P 2 Ru (found): C, 62.90 (63.01); H, 4.30 (4.71).
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