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Process for synthesizing 3-amino-5-methylpyrazole

A methylpyrazole and synthetic process technology, which is applied in the field of 3-amino-5-methylpyrazole synthetic process, can solve problems such as easy danger and difficult post-processing, and achieve high purity, mild reaction conditions, and easy synthesis The effect of simple process route

Inactive Publication Date: 2018-07-31
NANJING HABO MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this process is simple, it uses sodium hydride as alkali, which is prone to danger in the process of use, and the post-processing is difficult

Method used

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  • Process for synthesizing 3-amino-5-methylpyrazole

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 2000g of 3-aminobutene nitrile and 5L of ethanol into a 10L reaction flask, start stirring, stir until it is clear, add 2500g of 80% hydrazine hydrate, stir at room temperature for 10-20min., slowly heat to reflux, reaction temperature 85-95℃ ; Pay attention to a large amount of gas generation; heat preservation reaction for 1.5-2.5 hours, TLC monitoring, the reaction of the raw materials is complete; the reaction liquid is concentrated under reduced pressure at 50-60°C to 20%-30% of the original reaction liquid volume; After cooling, it becomes a pale yellow solid), 2230 g, yield 94.2%, detected by GC and HPLC, the purity of 3-amino-5-methylpyrazole is above 98%, and the single impurities are less than 0.5%.

Embodiment 2

[0021] As in Example 1, only the organic solvent ethanol was changed to the following substances to prepare 3-amino-5-methylpyrazole, and the yield was calculated;

[0022] Group

Embodiment 3

[0024] Same as Example 1, only changing the mass ratio of 3-aminobutenenitrile, organic solvent, and hydrazine hydrate to prepare 3-amino-5-methylpyrazole, and calculate its yield;

[0025] Group

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Abstract

The invention belongs to the technical field of synthesis of medicinal intermediates and particularly relates to a process for synthesizing 3-amino-5-methylpyrazole. The process comprises the following steps: (1) adding 3-aminocrotononitrile and an organic solvent into a reaction vessel, starting stirring, adding 80% hydrazine hydrate after a solution is clarified, heating the solution to 85 DEG Cto 95 DEG C, and carrying out a reaction for 1.5 to 2.5 hours while carrying out heat preservation; (2) subjecting the reaction solution prepared in the step (1) to depressurized concentration at thetemperature of 50 DEG C to 60 DEG C, and then, carrying out oil pump rectification, thereby preparing the 3-amino-5-methylpyrazole. According to the synthesis process, the 3-amino-5-methylpyrazole issynthesized in one step in the organic solvent by taking 3-aminocrotononitrile as a main raw material and taking hydrazine hydrate as adjuvants, the synthesizing process route is simple, superfluouswaste liquor cannot be produced, complicated aftertreatment is not required, the reaction conditions are mild, and the product is high in yield and high in purity.

Description

Technical field [0001] The invention belongs to the technical field of synthesis of pharmaceutical intermediates, and particularly relates to a synthesis process of 3-amino-5-methylpyrazole. Background technique [0002] Diabetes, as a worldwide disease, brings serious burden and pressure to patients, families and society. As a high-efficiency drug for the treatment of diabetes, Alatagliptin was immediately recognized by the affected patients due to its fast effect and long-lasting effect, which relieved the psychological and physical pain of the patients. At present, in the synthetic route of Alagliptin at home and abroad, the most commonly used intermediate is 3-amino-5-methylpyrazole. As an important intermediate in the synthesis of Alatagliptin, 3-amino-5-methylpyrazole has a direct impact on the quality and cost of the final drug. [0003] There are not many reports on its synthesis process at home and abroad. The main synthetic route is (1) Take 5-methylpyrazole as the mai...

Claims

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Application Information

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IPC IPC(8): C07D231/38
CPCC07D231/38
Inventor 崔家乙汪金柱张勇
Owner NANJING HABO MEDICAL TECH
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