Method for accelerating chemical reaction in microwave radiation condition
A technology of microwave radiation and chemical reaction, applied in the field of promoting chemical reaction under the condition of microwave radiation, can solve problems such as weak radiation absorption ability, and achieve the effects of good stability, increased superiority and scope of application, and promotion effect.
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Embodiment 1
[0013] Embodiment 1 promotes the hydrolysis reaction of ethyl benzoate under microwave radiation
[0014]
[0015] Efficient microwave absorber: SnO 2 (average particle size 50μm), dosage: 0.04g / mL.
[0016] Reaction system polarity: moderate.
[0017] In the 100mL reaction bottle, add 3.0g (20mmol) ethyl benzoate, 30mL 10% sodium hydroxide solution and 1.20g SnO 2 , 700w microwave (domestic pulse type, 20% duty cycle) irradiation for 42 minutes, after cooling to room temperature, the SnO 2 Filter out with a sand core funnel, rinse with dichloromethane, rinse with petroleum ether and sodium carbonate solution respectively, put the filtrate into a separatory funnel and let it stand, separate the water phase, acidify the water phase with hydrochloric acid, and dichloride The benzoic acid was extracted with methane, dried with anhydrous magnesium sulfate, filtered, and the solvent was removed to obtain 2.20 g of a white solid product with a yield of 90.16% and a melting poi...
Embodiment 2
[0018] Embodiment 2 promotes the hydrolysis reaction of ethyl benzoate under microwave radiation
[0019]
[0020] Efficient microwave absorber: Fe 3 o 4 (average particle size 1μm), dosage: 0.03g / mL.
[0021] Reaction system polarity: moderate.
[0022] In 100mL reaction bottle, add 3.0g (20mmol) ethyl benzoate, 30mL 10% sodium hydroxide solution and 0.9g Fe 3 o 4 , 700w microwave (domestic pulse, 20% duty cycle) irradiation for 40 minutes, after cooling to room temperature Fe 3 o 4 Filter out with a sand core funnel, rinse with dichloromethane, rinse with petroleum ether and sodium carbonate solution respectively, put the filtrate into a separatory funnel and let it stand, separate the water phase, acidify the water phase with hydrochloric acid, and dichloride The benzoic acid was extracted with methane, dried with anhydrous magnesium sulfate, filtered, and the solvent was removed to obtain 1.99 g of a white solid product with a yield of 81.56% and a melting point o...
Embodiment 3
[0023] Embodiment 3 promotes the reaction of anthracene and diethyl maleate Diels-Alder under microwave radiation
[0024]
[0025] High-efficiency microwave absorber: activated carbon (average particle size: 30μm), adding amount: 0.02g / mL.
[0026] Reaction system polarity: low.
[0027] Take 10.5g (61mmol) of diethyl maleate, 1.09g (6.1mmol) of anthracene, 0.4g of activated carbon, and 20mL of xylene in a 100mL flask. After shaking slightly, 500W microwave oven was continuously irradiated for 76min. After natural cooling to room temperature, 30 mL of dichloromethane was added to dissolve, the activated carbon was filtered out with a sand core funnel, and rinsed with dichloromethane, the solution was sampled for NMR analysis, and the conversion rate was 89.8%.
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