Synthesis method of p-toluenesulfonylurea
A technology of toluenesulfonylurea and p-toluenesulfonamide, which is applied in the field of synthesis of p-toluenesulfonylurea, can solve the problems of non-environmental protection, complicated preparation process, and by-products, and achieve non-toxic and pollution-free operating environment, easy operation The effect of simple steps and low production energy consumption
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Embodiment 1
[0025] A synthetic method for p-toluenesulfonylurea, comprising the steps of: adding p-toluenesulfonamide 171g (1mol), ethanol 150mL, sodium cyanate 78g (1.2mol), water 150mL in a there-necked flask, after stirring evenly, heating to Reflux at 78°C, keep warm for 8 hours until the raw materials basically react completely, cool down to below 30°C, filter to remove a small amount of unreacted raw materials that may exist, adjust the pH of the mother liquor to 2 with hydrochloric acid, and filter again to obtain , and dried at 50° C. to obtain 192.6 g of p-toluenesulfonylurea white powder, and the calculated yield was 90%.
[0026] The p-toluenesulfonylurea prepared in the present embodiment is carried out to the proton nuclear magnetic resonance spectrum test, and the spectrogram is as follows: figure 1 shown by figure 1 It can be seen that the product is p-toluenesulfonylurea.
[0027] The p-toluenesulfonylurea prepared in this embodiment is tested by high performance liquid ...
Embodiment 2
[0029] A synthetic method for p-toluenesulfonylurea, comprising the steps of: adding p-toluenesulfonamide 171g (1mol), ethanol 150mL, sodium cyanate 78g (1.2mol), water 150mL in a there-necked flask, after stirring evenly, heating to Reflux at 95°C, keep warm for 5 hours until the raw materials are basically reacted completely, cool down to below 30°C, filter to remove a small amount of unreacted raw materials that may exist, adjust the pH value of the filtered mother liquor to 2 with hydrochloric acid, and filter again to obtain p-toluene The sulfonylurea was dried at 50° C. to obtain 181.9 g of p-toluenesulfonylurea white powder, and the calculated yield was 85%.
[0030] The p-toluenesulfonylurea prepared in this example was subjected to a proton nuclear magnetic resonance spectrum test, and the peak position of the test result product was the same as in Example 1.
[0031] The p-toluenesulfonylurea prepared in this example was tested by high performance liquid chromatograp...
Embodiment 3
[0033] A synthetic method for p-toluenesulfonylurea, comprising the steps of: adding p-toluenesulfonamide 171g (1mol), ethanol 150mL, sodium cyanate 78g (1.2mol), water 150mL in a there-necked flask, after stirring evenly, heating to Reflux at 60°C, keep warm for 7 hours until the raw materials are basically reacted completely, cool down to below 30°C, filter to remove a small amount of unreacted raw materials that may exist, adjust the pH value of the filtered mother liquor to 1 with hydrochloric acid, and filter again to obtain p-toluene The sulfonylurea was dried at 50° C. to obtain 171.2 g of p-toluenesulfonylurea white powder, and the calculated yield was 80%.
[0034] The p-toluenesulfonylurea prepared in this example was subjected to a proton nuclear magnetic resonance spectrum test, and the peak position of the test result product was the same as in Example 1.
[0035] The p-toluenesulfonylurea prepared in this example was tested by high performance liquid chromatograp...
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