Method for preparing 3,5-dichloroaniline
A technology of dichloroaniline and dichlorobromobenzene, which is applied in the field of preparation of chlorine product 3,5-dichloroaniline, can solve the problems of difficult source of raw materials, harsh reaction conditions, low yield, etc. Simple, high-yield results
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Embodiment 1
[0020] Add 81 grams (0.5 mol) of 2,4-dichloroaniline, 200 grams of water, and 130 grams of 31% hydrochloric acid into a 1000 ml four-neck flask with a stirrer and a thermometer, and stir and add 80.4 grams of bromine (0.5 mol), and continued to stir for 40 minutes after dropping to obtain a reaction solution of 2-bromo-4,6-dichloroaniline hydrochloride, added 150 g (2.5 mol) of isopropanol, cooled to -10°C, and added dropwise (10 %) containing 35 grams of sodium nitrite (0.507 mol), after stirring for 50 minutes after dripping, the temperature was slowly raised to boiling at 5~15°C / 10 minutes, the azeotrope was collected, and the layers were separated to obtain 3,5- 110 grams of dichlorobromobenzene; add 110 grams of 3,5-dichlorobromobenzene, 150 grams of 28 (w / w)% ammonia water, and 5 grams (0.035 moles) of catalyst cuprous oxide into the autoclave, heat up, and control the temperature at 170 °C for 5 hours to complete the reaction. 77.8 g of 3,5-dichloroaniline was distille...
Embodiment 2
[0022] Add 81 grams (0.5 moles) of 2,4-dichloroaniline, 300 grams of water and 50 grams of 98% sulfuric acid into a 1000 ml four-necked flask with a stirrer and a thermometer, stir and add 80.4 grams (0.5 moles) of bromine dropwise, After dropping, continue stirring for 40 minutes to obtain a reaction liquid of 2-bromo-4,6-dichloroaniline hydrochloride, add 100 g (2.17 moles) of ethanol, cool to -10°C, add dropwise (15%) nitrous acid Aqueous solution of 35 grams of sodium (0.507 mol), after dripping and stirring for 50 minutes, slowly heat up to boiling at 5~15°C / 10 minutes, collect the azeotrope, stand for layer separation, and obtain 3,5-dichlorobromobenzene 108 grams; add 108 grams of 3,5-dichlorobromobenzene, 150 grams of 28 (w / w)% ammonia water, and 4.5 grams (0.031 moles) of catalyst cuprous oxide into the autoclave, raise the temperature, and react at 170°C for 5 hours. End the reaction. 75.2 g of 3,5-dichloroaniline was distilled, with a yield of 92%.
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