Preparation method of p-methoxybenzaldehyde
A technology of p-methoxybenzaldehyde and p-hydroxybenzaldehyde, which is applied in the field of preparation of p-methoxybenzaldehyde, can solve the problems of the number of varieties and the impact on product quality, and achieve low production equipment requirements, mild operating conditions, and side effects. The effect of less product
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Embodiment 1
[0013] A preparation method of p-methoxybenzaldehyde, using p-hydroxybenzaldehyde and dimethyl carbonate as raw materials, immobilized TEBA as catalyst, chloroform as solvent, adding sodium carbonate, and reacting under combined microwave and ultrasonic conditions ;Specific steps are as follows:
[0014] 1. In a three-necked flask, add 1mol p-hydroxybenzaldehyde, 1.35mol DMC, 4.8mol chloroform to dissolve, then add 0.015mol immobilized TEBA and 0.14mol sodium carbonate. Under microwave and ultrasonic conditions, reflux reaction. When the liquid in the bottle boils and there are reflux droplets dripping from the condenser, adjust the heat source to make the reflux rate normal, 2 drops per second. Continue heating to reflux, the microwave ultrasonic power is 650W and 550W respectively. 8 minutes.
[0015] 2. After the reaction is completed, cool to room temperature, filter and recover sodium carbonate, transfer the filtrate to a distillation flask, first remove the head under reduc...
Embodiment 2
[0017] A preparation method of p-methoxybenzaldehyde, the specific steps are as follows:
[0018] 1) In a three-necked flask, add 1mol p-hydroxybenzaldehyde, 1.55mol DMC, 4.9mol chloroform to dissolve, then add 0.01mol immobilized TEBA and 0.15mol sodium carbonate. Under microwave and ultrasonic conditions, reflux reaction. When the liquid in the bottle boils and there are reflux droplets dripping from the condenser, adjust the heat source to make the reflux rate normal, 2 drops per second. Continue heating to reflux, the microwave ultrasonic power is 675W and 600W respectively. Reflux for 10 minutes.
[0019] 2) After the reaction is complete, cool to room temperature, filter and recover sodium carbonate, transfer the filtrate to a distillation flask, first remove the head under reduced pressure, and then distill under reduced pressure, collect -0.098Mpa—0.1Mpa, and the fraction at 100~120℃ is the product P-Methoxybenzaldehyde. The content is 99.5% and the yield is 95.9%.
[002...
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