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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

Inactive Publication Date: 2020-10-09
JIANGSU UNIVERSITY OF TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the technical problems that the prior art method for preparing p-toluenesulfonylurea is not environmentally friendly, the preparation process is relatively complicated, and by-products are produced, a synthetic method of p-toluenesulfonylurea is provided

Method used

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  • Synthesis method of p-toluenesulfonylurea
  • Synthesis method of p-toluenesulfonylurea
  • Synthesis method of p-toluenesulfonylurea

Examples

Experimental program
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Effect test

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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Abstract

The invention relates to a synthesis method of p-toluenesulfonylurea. The synthesis method comprises the following steps: dissolving p-toluenesulfonamide and sodium cyanate in a mixed solution of water and ethanol to react, filtering after the reaction is finished, acidifying the filtered mother solution, and filtering again, thereby finally obtaining p-toluenesulfonylurea. According to the method, no by-product or ammonia gas is generated, the yield of the target product reaches 90% or above, the purity is larger than 99%, the process is simple, operation steps are simple and convenient, theoperation environment is non-toxic and free of pollution, no waste gas is generated, production energy consumption is low, the yield is high, and the method has very high popularization value.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a synthesis method of p-toluenesulfonylurea. Background technique [0002] In recent years, with the gradual improvement of living standards, the number of diabetic patients in the world has also shown a rising trend. According to the latest survey of "Prevalence and Control of Adult Diabetes in China", the prevalence of diabetes among adults aged 18 and above in China has reached as high as 11.6%, the prevalence of pre-diabetes has reached a staggering 50.1%. This means that 6 out of 10 adults have abnormal blood sugar. According to this ratio, the number of diabetic patients in my country has reached 114 million, and the number of pre-diabetics is close to 500 million. Diabetes has become one of the most important and difficult problems in our country. At present, oral hypoglycemic drugs commonly used in clinical practice mainly include α-glucosidase inhibitors, su...

Claims

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Application Information

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IPC IPC(8): C07C311/58C07C303/40C07C303/44
CPCC07C303/40C07C303/44
Inventor 孙丽侠李晶晶胡佳艳宋忠诚邱滢
Owner JIANGSU UNIVERSITY OF TECHNOLOGY
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