Chemical synthesis process of antibacterial agent spice carvacrol
A technology of carvacrol and antibacterial agent, applied in the field of chemical synthesis technology of antibacterial agent spice carvacrol, can solve the problems of high transportation storage and price, low final yield, low boiling point and the like
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Embodiment 1
[0021] Measure 500L of dichloromethane and add it to a 1000L reaction kettle with a stirring and cooling device, add 300kg of catalyst anhydrous aluminum trichloride, stir and cool down to -5°C, slowly add 100kg of o-cresol, and wait until the temperature of the reaction system reaches -5°C Finally, 72 kg of isopropanol was added dropwise, and the reaction was completed at -5 °C for 4 h. At room temperature, slowly add the reaction product into a reaction kettle with a stirrer equipped with 1200kg of crushed ice and stir until the ice melts
[0022] The ice was completely melted, left to stand, and the oil layer was separated, and the water layer was washed twice with 150L dichloromethane each time, and the separated oil layer was combined, concentrated at 55°C under normal pressure until no dichloromethane solvent was evaporated, and the fragrant 122.2 kilograms of crude product of cervacrol, carvacrol content 65.6% (HPLC assay). Vacuum distillation of 100 Pa, the fraction a...
Embodiment 2
[0024] Measure 500L of n-hexane and add it to a 1000L reaction kettle with a stirring and cooling device, add 300kg of catalyst anhydrous aluminum trichloride, stir and cool down to -5°C, slowly add 100kg of o-cresol, and wait until the temperature of the reaction system reaches -5°C , add 72kg of isopropanol dropwise, and react at -5 ℃ for 4h to end the reaction. At room temperature, slowly add the reaction product into a reaction kettle with a stirrer equipped with 1200kg of crushed ice and stir until the ice is completely melted, leave it to stand, separate the oil layer, and wash the water layer with 150L of dichloromethane each time for a total of two The second time, the separated oil layers were combined and concentrated under normal pressure at 70°C until no n-hexane (petroleum ether) solvent was evaporated to obtain 121.6 kg of crude carvacrol with a carvacrol content of 65.4% (as determined by HPLC). Vacuum rectification at 100 Pa vacuum degree collected the distilla...
Embodiment 3
[0026] Measure 500L of dichloromethane and add it to a 1000L reaction kettle with a stirring and cooling device, add 300.0kg of catalyst anhydrous ferric chloride, stir and cool down to -5°C, slowly add 100kg of o-cresol, and wait until the temperature of the reaction system reaches - After 5°C, 72kg of isopropanol was added dropwise, and reacted at -5°C for 4 hours to end the reaction. At room temperature, slowly add the reaction product into a reaction kettle with a stirrer equipped with 1200kg of crushed ice and stir until the ice is completely melted, let it stand, separate the oil layer, and wash the water layer with 150L of dichloromethane each time, a total of two The second time, the separated oil layers were combined and concentrated under normal pressure at 55°C until no dichloromethane solvent was evaporated to obtain 121.4 kg of carvacrol crude product with a carvacrol content of 65.4% (as determined by HPLC). Vacuum rectification at 100Pa vacuum degree collected t...
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