A kind of convenient preparation method of 2,6-dichlorophenylacetic acid
A technology of dichlorophenylacetic acid and malonate diester, which is applied in the direction of carboxylate preparation, carboxylate preparation, carboxylate preparation, etc., can solve the problem of high price of dichlorobenzyl alcohol, unfavorable industrial production, and poor operation safety and other issues, to achieve the effect of green process, low overall cost and high safety
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Embodiment 1
[0042] Embodiment 1: the preparation of 2,2,6,6-tetrachlorocyclohexanone
[0043] In the 500 milliliter four-necked flask that is connected with agitator, thermometer, reflux condenser and mass concentration of 10-30% sodium hydroxide aqueous solution absorption device, add 250 grams of dichloromethane, 9.9 grams (0.1 mole) cyclohexanone , 60.0 grams of potassium carbonate, heating, stirring between 30-45 ° C, slowly introducing chlorine gas, actually passing 33.5 grams of chlorine gas, reacting at 40-45 ° C for 5 hours until the reaction is complete, cooling to 20 ° C, filtering, and using the filter cake Dichloromethane washed 3 times, each 40 g. The dichloromethane filtrates were combined and the solvent was recovered by distillation to obtain 23.5 g of white powder solid 2,2,6,6-tetrachlorocyclohexanone with a yield of 99.8% and a gas phase purity of 99.5%.
Embodiment 2
[0044] Embodiment 2: the preparation of 2,2,6,6-tetrachlorocyclohexanone
[0045] In a 500 ml four-neck flask connected with a stirrer, a thermometer, a reflux condenser and a 10-30% sodium hydroxide aqueous solution absorption device, add 250 g of 1,2-dichloroethane, 9.9 g (0.1 mole ) cyclohexanone, 60.0 grams of potassium carbonate, heating, stirring at 40-50°C, slowly introducing chlorine gas, actually introducing 33.5 grams of chlorine gas, reacting at 45-50°C for 3 hours until the reaction is complete, cooling to 20°C, and filtering , The filter cake was washed 3 times with 1,2-dichloroethane, 40 g each time. The 1,2-dichloroethane filtrates were combined and the solvent was recovered by distillation to obtain 23.6 g of white powder solid 2,2,6,6-tetrachlorocyclohexanone with a yield of 99.9% and a gas phase purity of 99.7%.
Embodiment 3
[0046] Embodiment 3: the preparation of 2,2,6,6-tetrachlorocyclohexanone
[0047] In the 500 milliliter four-neck flask that is connected with agitator, thermometer, reflux condenser and mass concentration of 10-30% sodium hydroxide aqueous solution absorption device, add 250 gram of dichloromethane, 9.9 gram (0.1 mole) cyclohexanone, 50.0 grams of sodium carbonate, heated, stirred at 30-45 °C, slowly introduced chlorine gas, actually introduced 33.5 grams of chlorine gas, reacted at 40-45 °C for 5 hours until the reaction was complete, cooled to 20 °C, filtered, and the filter cake was washed with two Chloromethane washed 3 times, each 40 g. The dichloromethane filtrates were combined and the solvent was recovered by distillation to obtain 23.1 g of white powder solid 2,2,6,6-tetrachlorocyclohexanone with a yield of 97.9% and a gas phase purity of 99.8%.
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