Method for preparing 1,2,3-thiadiazole-4-carboxylic acid
A technology of thiadiazole and dicarboxylic acid, which is applied in the field of compound synthesis, can solve the problems that the synthesis process cannot be enlarged and industrialized, and the synthesis rate is low, and achieve the effect of low price, high synthesis rate and easy availability of raw materials
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[0020] Into a 10L four-necked flask, add diaminomaleic cyanide: 410g, THF: 3.79L, triethylamine: 1.718kg, cool down to 0°C and slowly add thionyl chloride: 918.68g, dropwise, continue stirring After 6 hours, filter, wash the filter cake with THF, combine the washing liquid with the filtrate, spin dry (rotate to dryness), add 1.5 L of dichloroethane and 5 L of water, and steam distill to obtain 300 g of light yellow solid. Detection: HPLC 220nm 98%, yield of 4,5-dicyano-1,2,3-thiadiazole: 58.1%.
[0021] The reaction formula is:
[0022]
[0023] In a 2L four-neck flask, add water: 600g, slowly drop concentrated sulfuric acid: 600g, make 50% sulfuric acid aqueous solution, then add 4,5-dicyano-1,2,3-thiadiazole: 300g, React at 120°C for 12 hours, cool down to 0°C, stir for 2 hours, and filter to obtain 337.7g of white solid 1,2,3-thiadiazole 4,5-dicarboxylic acid, yield: 88%.
[0024] The reaction formula is:
[0025]
[0026] Put 250g of the white solid into a 500ml f...
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