A kind of preparation method of 4-amino-3-isopropyl-1,2,4-triazolin-5-one
An isopropyl, triazoline technology, applied in the field of organic chemical synthesis, can solve the problems of large investment, harsh operating environment, high requirements for safety facilities and production equipment and facilities, achieve simple and safe operation, avoid the use of toxic reagents, avoid Effects of the use of the potent drug phosgene
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Embodiment 1
[0036] This embodiment provides a preparation method of 4-amino-3-isopropyl-1,2,4-triazolin-5-one:
[0037] Put 100 mL of ethanol into a 500 mL four-necked flask, turn on stirring, put in 86.4 g (0.95 mol) of carbohydrazide and 79.6 g (0.57 mol) of potassium carbonate, and heat up to reflux. Under reflux conditions, 115.0 g (0.98 mol) of ethyl isobutyrate was added dropwise, and the dropwise addition was completed in about 1 hour. Incubate at 70-75°C for 3 hours, complete the reaction, remove 80 ml of ethanol, then add 100 mL of water to the reaction solution, slowly cool down to 0°C for crystallization, filter, and dry to obtain 103.6 g of an off-white solid, the target product, with a purity of 98.0% and a yield. 75.2%.
Embodiment 2
[0039] This embodiment provides a preparation method of 4-amino-3-isopropyl-1,2,4-triazolin-5-one:
[0040] 100 mL of toluene was put into a 500 mL four-necked flask, stirring was started, 86.4 g (0.95 mol) of carbohydrazide and 26.4 g (1.09 mol) of lithium hydroxide were put in, and the temperature was raised to reflux. 102.1 g (0.99 mol) of methyl isobutyrate was added dropwise at reflux temperature, and the dropwise addition was completed in about 2 hours. The temperature was kept at 105-110°C for 2 hours, the reaction was completed, the toluene was removed under negative pressure, 100 mL of water was then put in, cooled to 0°C for crystallization, filtered, and dried to obtain 100.7 g of a white solid, the target product, with a purity of 98.0% and a yield of 73.1%.
Embodiment 3
[0042] This embodiment provides a preparation method of 4-amino-3-isopropyl-1,2,4-triazolin-5-one:
[0043]Drop into 100mL of water in a 500mL four-necked flask, turn on stirring, drop into 84.6g (0.93mol) carbohydrazide and 86.3g (0.97mol) isobutyric acid, be warming up to 60~65 ℃, and be incubated and reacted at this temperature for 5 hours , then drop 40.0g (0.99mol) sodium hydroxide into the reaction solution, continue to be warming up to reflux, and be incubated for about 3 hours under reflux conditions, the reaction is completed, slowly cooled to 0 ° C for crystallization, filtered, and dried to obtain a white solid that is The target product is 100.6 g, the purity is 98.3%, and the yield is 74.8%. The resulting product was analyzed and the results were as follows Figure 1-4 shown, where figure 1 is the liquid phase mass spectrometry (LC-MS) spectrum in positive ion mode, figure 2 For the negative ion mode liquid phase mass spectrometry (LC-MS) spectrum; image 3 I...
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