Process for removing N-nitroso-pendimethalin from pendimethialin
A technology of nitroso pendimethalin and pendimethalin, applied in chemical instruments and methods, preparation of amino compounds from amines, preparation of amino compounds, etc., can solve the problems of reducing the content of nitrosamines and not being able to use them , to achieve the effects of lowering the denitration temperature, reducing the amount of removing agent, and lowering the reaction temperature
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[0030] Example 1:
[0031] 6g (0.02mol) of pendimethalin containing a certain amount of pendimethalin (content 30%) detected by HPLC was dissolved in 30g (24ml) 1,2-dichloroethane and stirred Place it in a three-necked flask with a condenser, a thermometer and a stirring and heating device, then add 12g of concentrated hydrochloric acid (10ml), gradually increase the temperature to 75℃, and react for 1h; then add 1.2g FeCl 2 ·4H 2 O (0.006 mol), continue to react at 75°C for 3 hours, and then stop stirring. Sampling was tested by HPLC, and the content of N-nitrosodimethalin was less than 100 ppm.
[0032] Liquid chromatography analysis conditions: C18 column (150mm×4mm), mobile phase: acetonitrile: water = 80: 20 (v / v), flow rate 1.0mL / min, detection wavelength 254nm, pendimethalin retention time 5.93min , N-nitroso pendimethalin retention time is 3.36min, and the area is normalized and quantified (the same below).
Example Embodiment
[0033] Example 2:
[0034] Dissolve 6g (0.02mol) of pendimethalin containing a certain amount of pendimethalin (content 30%) detected by HPLC in 6g (5ml) 1,2-dichloroethane, start Stir and place it in a three-necked flask with condenser, thermometer and stirring heating device, then add 3g (2.5ml) concentrated hydrochloric acid, gradually increase the temperature to 75℃, react for 1h; then add 0.3g FeCl 2 ·4H 2 O (0.0015 mol), continue to react at 75° C. for 3 hours and then stop stirring. After sampling, the content of N-nitrosodimethyldimethalin is less than 100 ppm. (Analysis method is the same as in Example 1).
Example Embodiment
[0035] Example 3:
[0036] 6g (0.02mol) of pendimethalin containing a certain amount of pendimethalin (content 30%) detected by HPLC was dissolved in 60g (47.7ml) 1,2-dichloroethane, Start stirring and place it in a three-necked flask with condenser, thermometer and stirring heating device, then add 15g (12.6ml) concentrated hydrochloric acid, gradually increase the temperature to 75℃, react for 1h; then add 6g FeCl 2 ·4H 2 O (0.03 mol), continue to react at 75°C for 3 hours, and then stop stirring. Sampling was tested by HPLC, and the content of N-nitrodimethalin was less than 100 ppm. (Analysis method is the same as in Example 1).
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