Synthesis process of 1, 2, 3-trimethoxy benzene
A technology of trimethoxybenzene and synthesis process, which is applied in the directions of ester reaction preparation of ether, ether preparation, organic chemistry, etc., to achieve the effects of low synthesis cost, simple operation and wide source of raw materials
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Embodiment 1
[0036] In actual production, put the calculated 150 kg of guaiacol into the reactor, 100 kg of acetyl chloride into the high-level tank, slowly add acetyl chloride dropwise under stirring, and pay attention to the absorption of HCl in the tail gas as the dropwise addition proceeds. At the same time, during the process of adding acetyl chloride dropwise, the temperature in the reactor is controlled at -5°C; at the end of the dropwise addition, the holding temperature is controlled at 0°C, and the holding time is 4 hours until the reaction is complete. Judgment, the reaction is considered complete until the raw material point completely disappears. After the reaction is complete, 400 kg of o-xylene and 160 kg of aluminum chloride are put into the mixture, and the rearrangement reaction is carried out at 100° C. for 5 hours of heat preservation and reflux. The end point of the reaction was judged by thin-layer chromatography (TLC), and the reaction was considered complete until t...
Embodiment 2
[0038]In actual production, put the calculated 150 kg of guaiacol into the reactor, 96 kg of acetyl chloride into the high-level tank, slowly add acetyl chloride dropwise under stirring, and pay attention to the absorption of HCl in the tail gas as the dropwise addition proceeds. At the same time, during the process of dropping acetyl chloride, the temperature in the reactor is controlled at 20°C; at the end of the dropwise addition, the holding temperature is controlled at 30°C, and the holding time is 2 hours until the reaction is complete, and the end point of the reaction is judged by thin layer chromatography (TLC). , until the raw material point completely disappears, the reaction is considered complete. After the reaction is complete, 380 kg of o-xylene and 155 kg of aluminum chloride are put into the mixture, and the rearrangement reaction is carried out at 150° C. for 2 hours of heat preservation and reflux. The end point of the reaction was judged by thin-layer chrom...
Embodiment 3
[0040] In actual production, put the calculated 150 kg of guaiacol into the reactor, 105 kg of acetyl chloride into the high level tank, slowly add acetyl chloride dropwise under stirring, and pay attention to the absorption of HCl in the tail gas as the dropwise addition proceeds. At the same time, during the process of adding acetyl chloride dropwise, the temperature in the reactor is controlled at 10°C; at the end of the dropwise addition, the holding temperature is controlled at 15°C, and the holding time is 3 hours until the reaction is complete, and the end point of the reaction is judged by thin layer chromatography (TLC). , until the raw material point completely disappears, the reaction is considered complete. After the reaction is complete, 450 kg of o-xylene and 180 kg of aluminum chloride are put into the mixture, and the rearrangement reaction is refluxed at 120° C. for 3 hours of heat preservation and reflux. The end point of the reaction was judged by thin-layer...
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