Chemical synthesis process of 4-chloro-2-fluoro nitrobenzene
A technique for the synthesis of fluoronitrobenzene and its synthesis method, which is applied in the field of synthesizing 4-chloro-2-fluoronitrobenzene, can solve the problems that the purity of industrial products is only 90%, nitrochlorobenzene is not easy to obtain, and the price is high. Effects of mild conditions, few by-products, and simple operation
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Embodiment 1
[0013] 5-Chloro-2-nitroaniline hexafluorophosphate diazonium salt: In a 200ml three-necked flask, add 20.7g (0.12mol) 5-chloro-2-nitroaniline and 120ml 36% concentrated hydrochloric acid, stir, and cool in an ice-water bath to 5-10°C, then add dropwise 15ml of aqueous solution containing 8.8g (0.13mol) sodium nitrite within 60min at this temperature, and continue to stir and react at 5-10°C for 1.5h after the addition is complete. Remove a small amount of insoluble matter by suction filtration, and slowly add the filtrate to 63.5 g of 40% hexafluorophosphoric acid aqueous solution under cooling in an ice-water bath, control the reaction temperature at 5-10°C and stir for 30 minutes, then suction filtration, and successively wash with a little cold water, methanol / ether ( 1:10) solution and diethyl ether, and vacuum-dried to obtain 32.9 g of light yellow powdered diazonium hexafluorophosphate, with a yield of 83%.
Embodiment 2
[0015] 5-Chloro-2-nitroaniline diazonium hexafluorophosphate: except that the reaction temperature was controlled at -10 to 5°C, other operating conditions were the same as in Example 1, and 27.8 g of light yellow powder diazonium hexafluorophosphate was obtained. , yield 71%.
Embodiment 3
[0017] 5-Chloro-2-nitroaniline diazonium hexafluorophosphate: except that the reaction temperature was controlled at 15-20°C, other operating conditions were the same as in Example 1, and 24.5 g of light yellow powdered diazonium hexafluorophosphate was obtained. Yield 63%.
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