Synthesis process of hydroxybenzene ether (III)
A technology for the synthesis of hydroxyphenyl ethers, which is applied in the field of synthesis of hydroxyphenyl ethers, can solve the problems of low utilization rate of monochloromethane, poor reaction selectivity, serious environmental pollution, etc., and achieve the reduction of process wastewater, stable quality, and high efficiency. less effect
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Embodiment 1
[0057] (1) Prepare the alkylation reaction solution:
[0058] Reaction solution-1: 376g (3.08mol) o-hydroxybenzaldehyde I mixed with 560g toluene as reaction solution-1;
[0059] Reaction solution-2: 585.5g of 30% liquid caustic soda mixed with 5g of tetrabutylammonium bromide as reaction solution-2;
[0060] Reaction solution-3: 517g (3.36mol) diethyl sulfate was used as reaction solution-3;
[0061] (2) Synthesis of o-ethoxybenzaldehyde II:
[0062] Use the pump-1 with a flow rate of 50mL / min to inject the reaction solution-1 into the microreactor, use the pump-2 to inject the reaction solution-2 into the microreactor, and use the pump-3 to inject the reaction solution-3 into the microreactor Among them, the injection speed of pump-2 and pump-3 is adjusted according to the injection speed of pump-1, so as to ensure that the three reaction solutions are injected simultaneously, and the reaction is carried out at 80±5°C.
[0063] After the reaction is completed, the layers ...
Embodiment 2
[0071] (1) Prepare the alkylation reaction solution:
[0072] Reaction solution-1: 376g (3.08mol) o-hydroxybenzaldehyde I mixed with 376g water as reaction solution-1;
[0073] Reaction solution-2: 585.5g of 30% liquid caustic soda mixed with 18.8g of benzyltriethylammonium chloride as reaction solution-2;
[0074] Reaction solution-3: 232.8g (1.85mol) dimethyl sulfate as reaction solution-3;
[0075] (2) Synthesis of o-methoxybenzaldehyde II:
[0076] Use the pump-1 with a flow rate of 100mL / min to inject the reaction solution-1 into the microreactor, use the pump-2 to inject the reaction solution-2 into the microreactor, and use the pump-3 to inject the reaction solution-3 into the microreactor Among them, the injection speeds of pump-2 and pump-3 were adjusted according to the injection speed of pump-1 to ensure that the three reaction solutions were fed simultaneously and reacted at 60°C.
[0077] After the reaction was completed, the layers were separated, and the alka...
Embodiment 3
[0085] (1) Prepare the alkylation reaction solution:
[0086] Reaction solution-1: 376g (3.08mol) p-hydroxybenzaldehyde I mixed with 276g toluene and 100g water as reaction solution-1;
[0087] Reaction solution-2: 585.5g 30% liquid caustic soda mixed with 1.88g PEG400 as reaction solution-2;
[0088] Reaction solution-3: 310.5g (2.46mol) dimethyl sulfate was used as reaction solution-3;
[0089] (2) Synthesis of p-methoxybenzaldehyde II:
[0090] Use the pump-1 with a flow rate of 20mL / min to inject the reaction solution-1 into the microreactor, use the pump-2 to inject the reaction solution-2 into the microreactor, and use the pump-3 to inject the reaction solution-3 into the microreactor Among them, the injection speeds of pump-2 and pump-3 were adjusted according to the injection speed of pump-1, so as to ensure that the three reaction solutions were fed simultaneously and reacted at 100°C.
[0091] After the reaction is completed, the layers are separated, and the lowe...
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