A kind of method for catalyzing and synthesizing pseudo-ionone by alkaline immobilized ionic liquid
A pseudo-ionone, ionic liquid technology, applied in chemical instruments and methods, preparation of organic compounds, catalysts for physical/chemical processes, etc., can solve problems such as yield impact, product color difference, corrosion, etc., to avoid catalysts Loss, product purity, high product yield effect
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Embodiment 1
[0016] Example 1: Preparation of Immobilized Ionic Liquid A
[0017] In a 150 mL three-necked flask, 41.1 g (0.5 mol) of 1-methylimidazole and 53.5 g (0.5 mol) of vinyl bromide were added, respectively, and the reaction was stirred at 70 °C for 5 h. After the reaction was completed, it was cooled to room temperature to obtain a colorless sticky substance. thick liquid. After extraction with ether for 20 mL×3 times, and vacuum drying, 94.5 g of 1-vinyl-3-methylimidazolium bromide salt was obtained as a colorless viscous liquid.
[0018] Into a 250 mL three-necked flask were added 94.5 g (0.5 mol) of the 1-vinyl-3-methylimidazolium bromide ionic liquid prepared above, 22.0 g (0.55 mol) of NaOH powder, and 100 mL of dichloromethane. Stir for 24 h. After the reaction was completed, the NaBr solid and excess NaOH solid were removed by suction filtration. The filtrate was distilled under reduced pressure to remove dichloromethane to obtain the vinyl-containing ionic liquid interm...
Embodiment 2
[0020] Example 2: Preparation of Immobilized Ionic Liquid B
[0021] In a 250 mL three-necked flask, 55.6 g (0.5 mol) of N-vinylpyrrolidone, 22.0 g (0.55 mol) of NaOH powder, and 100 mL of dichloromethane were added, and the mixture was stirred at room temperature for 24 h. After the reaction was completed, the excess NaOH solid was removed by suction filtration. The filtrate was distilled under reduced pressure to remove dichloromethane to obtain the intermediate [Vnmp]OH ionic liquid, and the mass yield of the intermediate product was 99%.
[0022] Weigh 12.8 g (0.1 mol) of the intermediate prepared above, dissolve it with 100 mL of absolute ethanol, then weigh 91.2 g (0.3 mol) of styrene and 1.8 g (11 mmol) of initiator AIBN in 250 mL of The reaction was heated under reflux in a three-necked round-bottomed flask, and stirred magnetically for 24 hours. After the reaction was completed, it was cooled to room temperature to obtain a white solid. The white solid was filtered o...
Embodiment 3
[0023] Example 3: Preparation of Immobilized Ionic Liquid C
[0024] In a 150 mL three-necked flask, 50.6 g (0.5 mol) of triethylamine and 53.5 g (0.5 mol) of vinyl bromide were added, and the reaction was stirred at 70 °C for 5 h. After the reaction was completed, it was cooled to room temperature to obtain a colorless viscous liquid . After extraction with ether 20 mL×3 times, and vacuum drying, 104.1 g of N,N,N-triethylethylene bromide was obtained as a colorless viscous liquid.
[0025] Into a 250 mL three-necked flask were added 104.1 g (0.5 mol) of N,N,N-triethylethylene bromide prepared above, 22.0 g (0.55 mol) of NaOH powder, and 100 mL of dichloromethane, and stirred at room temperature for 24 h. After the reaction was completed, the NaBr solid and excess NaOH solid were removed by suction filtration. The filtrate was distilled under reduced pressure to remove dichloromethane to obtain the vinyl-containing ionic liquid intermediate [Vtea]OH, and the mass yield of t...
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