Preparation method of foramsulfuron
A technology of foramsulfuron and methylsulfonamide, which is applied in the field of foramsulfuron-methyl preparation, can solve the problems of environmental pollution, a large amount of waste acetic acid, etc., achieve high formylation reaction yield, avoid impurities, and simple operation
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Embodiment 1)
[0018] This embodiment is the method for preparing 2-dimethylaminocarbonyl-5-formylaminophenylsulfonamide from 2-dimethylaminocarbonyl-5-aminophenylsulfonamide:
[0019] Add 50.0g of 2-dimethylaminocarbonyl-5-aminophenylsulfonamide, 2.5g of potassium tert-butoxide, and 300mL of ethyl formate into the reaction device, and first stir the reaction at a temperature of 20-25°C 2h, and then raise the temperature to 60±2°C for 5h.
[0020] After the reaction, it was cooled, filtered with suction, and dried to obtain 50.2 g of white solid 2-dimethylaminocarbonyl-5-formylaminophenylsulfonamide, with a yield of 90.0% and a purity of 97.0% (HPLC).
Embodiment 2~ Embodiment 5)
[0022] The method of each embodiment is basically the same as that of Example 1, and the differences are shown in Table 1.
[0023] Table 1
[0024]
Embodiment 6)
[0026] This embodiment is the method for preparing foramsulfuron-methyl from 2-dimethylaminocarbonyl-5-formylaminophenylsulfonamide and phenyl dimethoxypyrimidine carbamate:
[0027] 61.4 g of 2-dimethylaminocarbonyl-5-formylaminophenylsulfonamide, 24 g of triethylamine, 300 mL of acetonitrile, and 65.1 g of 4,6-dimethoxypyrimidine 2-carbamate phenyl Add it to the reaction device, stir and heat up to 50±2°C, and react for 5h.
[0028] After the reaction, 200mL of acetonitrile was distilled off under reduced pressure, cooled, an appropriate amount of ice water was added, and then hydrochloric acid was added dropwise to adjust the pH=3, suction filtered, washed with water, and dried to obtain 92.2 g of off-white solid foramsulfuron, with a yield of 90.0% , with a purity of 95.3% (HPLC).
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