2-mercapto-5-methyl-1,3,4-thiadiazole compound and synthesis method thereof
A technology of thiadiazoles and synthetic methods, which is applied in the direction of organic chemistry, can solve the problems of harsh reaction conditions, complex synthesis steps, and difficulty in realization, and achieve the effects of reducing the formation of impurities, increasing heat dissipation efficiency, and reducing side reactions
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Embodiment 1
[0043] The embodiment of the present invention provides a synthesis method of 5-amino-3-methyl-1,2,4-thiadiazole, comprising:
[0044]At room temperature (about 25°C), add 2-iminopropanenitrile (136g, 2mol) into acetone (500ML), and stir evenly; lower the temperature and keep it below 10°C; under continuous stirring, Hydrogen sulfide (31 g) was added to the mixed solution at a constant rate (700 rpm) within 10 minutes, and stirred at a speed of 700 rpm for 0.5 h, the solution became milky; the mechanical stirring speed was increased to 850 rpm , Pyridine (13.6 g, 10% mass of aminopropionitrile) was added quickly at one time, and the reaction temperature was controlled to be 5° C., the solution gradually became clear, and precipitation occurred. Keep the reaction temperature at 5°C, add hydrogen sulfide (20g) again, continue stirring for 0.5h, collect the precipitate, wash thoroughly with acetone, and dry to obtain the desired product 5-amino-3-methyl-1,2,4-thiadi azole. The ...
Embodiment 2- Embodiment 10
[0046] Embodiment 2-embodiment 10 provides a kind of synthetic method of 5-amino-3-methyl-1,2,4-thiadiazole, and this synthetic method and the 5-amino-3-methyl-1 that embodiment 1 provides The operation of the synthetic method of 1,2,4-thiadiazole is the same, the difference is that the operating conditions are changed, as follows:
[0047] The reaction conditions and the results of embodiment 2-embodiment 4 are shown in the table below:
[0048]
[0049]
[0050] The reaction conditions and the results of embodiment 5-embodiment 7 are shown in the table below:
[0051]
[0052] The reaction conditions and the results of embodiment 8-10 are shown in the following table:
[0053]
[0054] For the HPLC analysis diagram of 5-amino-3-methyl-1,2,4-thiadiazole prepared in Example 2-Example 4, see Figure 2-4 .
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