A kind of method for bimetallic oxidation catalyzed synthesis of trimethylhydroquinone diester
A technology of trimethylhydroquinone diester and catalyst, which is applied in the oxidation preparation of carbonyl compounds, chemical instruments and methods, and the preparation of organic compounds, etc. It can solve the problems of low product selectivity, influence of equipment and pipeline operation, and wastewater treatment, etc. problem, to achieve low price, avoid the use of strong acid catalyst, and react to the effect of green environmental protection
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Embodiment 1
[0047] Preparation of Rh catalyst:
[0048] Weigh 58.2g of rhodium trichloride trihydrate (purity of 39%wt) and 35.2g of 2,2-bipyridine respectively, add them into the reaction flask, then add 100ml of chloroform, replace with nitrogen and heat to 70°C and reflux for 5h to stop the reaction and cooled to room temperature, then suction filtered, washed three times with 20 ml of chloroform to obtain a crude Rh catalyst, and finally recrystallized with 150 ml of petroleum ether to obtain a Rh catalyst with a yield of 75% and a purity of 98.5%.
[0049] To prepare trimethylhydroquinone diester:
[0050] 15.2g of 2,6-dimethylphenol was added to the reaction flask, 0.008g of palladium acetate and 0.007g of the Rh catalyst prepared above were added, then 120ml of ethanol was added, and nitrogen was replaced three times. After nitrogen replacement, 23.6g of trimethylamine and 8.5g of hydrogen peroxide were added, and the temperature was raised to 60°C for reaction. After 0.5h of reac...
Embodiment 2
[0052] Preparation of Rh catalyst:
[0053] Weigh 58.2g of rhodium trichloride trihydrate (purity of 39%wt) and 40.1g of 2,2-bipyrimidine respectively, add them into the reaction flask, then add 100ml of tert-butanol, heat to 85°C for reflux for 4h after nitrogen replacement, The reaction was stopped and cooled to room temperature, followed by suction filtration, washed three times with 30 ml of tert-butanol to obtain crude Rh catalyst, and finally recrystallized with 200 ml of ether to obtain Rh catalyst with a yield of 73% and a purity of 95.1%.
[0054] To prepare trimethylhydroquinone diester:
[0055]12.2 g of 2,6-dimethylphenol was added to the reaction flask, 0.006 g of palladium acetate and 0.005 g of the Rh catalyst prepared above were added, and then 120 ml of acetone was added, and nitrogen was replaced three times. After nitrogen replacement, 28.5g of 1,2-dimethylpiperazine and 37.2g of sodium hypochlorite were added, and the temperature was raised to 110°C for re...
Embodiment 3
[0057] Preparation of Rh catalyst:
[0058] Weigh 58.2g of rhodium trichloride trihydrate (purity of 39%wt) and 39.5g of 2,3-bipyridine respectively, add them into the reaction flask, then add 150ml of chloroform, replace with nitrogen and heat to 100°C for reflux for 3h to stop the reaction and cooled to room temperature, then suction filtered, washed three times with 20 ml of chloroform to obtain a crude Rh catalyst, and finally recrystallized with 200 ml of acetone to obtain a Rh catalyst with a yield of 82% and a purity of 97.8%.
[0059] To prepare trimethylhydroquinone diester:
[0060] 12.2 g of 2,6-dimethylphenol was added to the reaction flask, 0.008 g of palladium acetate and 0.004 g of the Rh catalyst prepared above were added, and then 150 ml of methanol was added, and nitrogen was replaced three times. After nitrogen replacement, 50g of 1,2-dimethylpiperazine and 30.0g of hypochlorous acid were added, and the temperature was raised to 80°C for reaction. After 0.5...
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