The preparation method of iodosulfuron sodium salt intermediate
A technology of iodosulfuron-methyl sodium salt and intermediate is applied in the field of preparation of iodosulfuron-methyl sodium salt intermediate 6-iodosaccharin, and can solve the problems of high cost of wastewater treatment, non-compliance with economic requirements, non-compliance with environmental protection requirements and the like , to achieve the effect of avoiding decomposition and hydrolysis, high product yield and low environmental protection cost
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Embodiment 1)
[0030] The reaction formula of the present embodiment is as follows:
[0031] .
[0032] The concrete method of this embodiment is as follows:
[0033] Add 20g (0.101mol) of 6-aminosaccharin, 17.6g (0.106mol) of potassium iodide, 6.4g (0.107mol) of acetic acid and 100g of toluene into a 500mL reaction bottle, and drop 11.8g (0.101mol) of isoamyl nitrite at about 10°C mol), reacted at 20°C for 2 hours after dropping, then added 20g of water, stirred for 10 minutes, allowed to stand for stratification, added 15g of sodium carbonate aqueous solution with a concentration of 10wt% to the organic layer, stirred for 10 minutes, stood for stratification, The organic layer was precipitated to obtain 28.1 g of 6-iodosaccharin with a content of 96% and a yield of 90.0%.
Embodiment 2)
[0035] The reaction formula of the present embodiment is as follows:
[0036] .
[0037] The concrete method of this embodiment is as follows:
[0038] Add 20g (0.101mol) of 6-aminosaccharin, 17.6g (0.106mol) of potassium iodide, 6.4g (0.107mol) of acetic acid and 100g of toluene into a 500mL reaction bottle, and add 10.4g (0.101mol) of n-butyl nitrite dropwise at about 10°C mol), reacted at 20°C for 2 hours after dropping, then added 20g of water, stirred for 10 minutes, allowed to stand for stratification, added 15g of sodium carbonate aqueous solution with a concentration of 10wt% to the organic layer, stirred for 10 minutes, stood for stratification, The organic layer was precipitated to obtain 27.5 g of 6-iodosaccharin with a content of 95% and a yield of 88.1%.
Embodiment 3)
[0040] The reaction formula of the present embodiment is as follows:
[0041] .
[0042] The concrete method of this embodiment is as follows:
[0043] Add 20g (0.101mol) of 6-aminosaccharin, 17.6g (0.106mol) of potassium iodide, 6.4g (0.107mol) of acetic acid and 100g of toluene into a 500mL reaction bottle, and drop 9.0g (0.101mol) of isopropyl nitrite at about 10°C mol), reacted at 20°C for 2 hours after dropping, then added 20g of water, stirred for 10 minutes, allowed to stand for stratification, added 15g of sodium carbonate aqueous solution with a concentration of 10wt% to the organic layer, stirred for 10 minutes, stood for stratification, The organic layer was precipitated to obtain 26.5 g of 6-iodosaccharin with a content of 95% and a yield of 84.9%.
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