Low-voltage hydrogenation process of isopropyl pyrazolone

A technology of propyl pyrazolone and pyrazolone, which is applied in the field of chemical synthesis preparation technology, can solve problems such as safety and cost, and achieve the effects of fast reaction speed, cost reduction, and reduction of equipment requirements

Inactive Publication Date: 2008-12-24
SHANDONG XINHUA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] The technical problem to be solved by the present invention is to provide a new process for synthesizing isopropyl pyrazolone to solve the problems of environmental protection, safety and cost in the existing process

Method used

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  • Low-voltage hydrogenation process of isopropyl pyrazolone

Examples

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Effect test

Embodiment 1

[0027] Example 1: Put 30g of pyrazolone, 100g of acetone, and 1.5g of Raney nickel into the hydrogenation reaction kettle together. After four times of replacement with nitrogen, four times of replacement with hydrogen, the hydrogen is discharged to <0.1Mpa, and then the temperature is raised to At about 75°C, raise the pressure to 0.3Mpa to start the reaction, keep the pressure in the kettle at 0.3Mpa, and the reaction temperature at 80°C. After the reaction was completed, the reaction solution was lowered to 60°C, and the reaction solution was filtered out with a filter press, the temperature of the reaction solution was lowered, and it was crystallized at 0-5°C and then filtered to obtain 35 g of white powdery solid isopyrazolone. Yield 93.99%, content 99.21%.

Embodiment 2

[0028] Example 2: Put 50g of pyrazolone, 165g of acetone, and 2.5g of Raney's nickel into the hydrogenation reactor. After four times of nitrogen replacement, four times of hydrogen replacement, the hydrogen is discharged to <0.1Mpa, and then the temperature is raised to At about 75°C, raise the pressure to 0.32Mpa to start the reaction, keep the pressure in the kettle at 0.32Mpa, and the reaction temperature at 82°C. After the reaction was completed, the reaction solution was lowered to 60°C, and the reaction solution was filtered out with a filter press, the temperature of the reaction solution was lowered, and the crystallization was carried out at 0-5°C, followed by filtration to obtain 59 g of white powdery solid isopyrazolone. Yield 95.06%, content 99.03%.

Embodiment 3

[0029] Example 3: 50g of pyrazolone, 140g of acetone, and 2g of Raney nickel were put into the hydrogenation reaction kettle together, and after four times of replacement with nitrogen, four times of replacement with hydrogen, the hydrogen was discharged to <0.1Mpa, and then the temperature was raised to 75 ℃, raise the pressure to 0.3Mpa, start the reaction, keep the pressure in the kettle at 0.3Mpa, and the reaction temperature at 85℃. After the reaction was completed, the reaction liquid was lowered to 60°C, and the reaction liquid was filtered out with a filter press, the temperature of the reaction liquid was lowered, and the temperature of the reaction liquid was crystallized at 0-5°C, and then filtered to obtain 45 g of white powdery solid isopyrazolone. Yield 90.63%, content 99.48%.

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Abstract

The invention provides a novel low-pressure hydrogenation technique for synthesizing isopropyl pyrazolone. Acetone and pyrazolone are condensed and hydrogenated, the acetone is taken as a solvent and Raney nickel is taken as a catalyst. The technique adopts the Raney nickel as the catalyst in the hydrogenation reaction, thereby achieving the same effect of using noble metal catalyst, lowering the cost, avoiding the pollution caused by the zinc powder process production and having the characteristics of cleanness and environment protection. The acetone is taken as the solvent of the hydrogenation reaction and serves as both the reactant and the solvent, thereby greatly increasing the concentration of the reactant and making the hydrogenation reaction easier; and the reaction pressure is low, the reaction speed is fast, the time is short and the product quality is good. Meanwhile, the solvent can be reclaimed and used intervalically, thereby having obvious cost advantage and the characteristics of low cost and environment protection. The pressure of the hydrogenation reaction is reduced, thereby increasing the safety coefficient of the reaction and reducing the requirement on a device.

Description

technical field [0001] The invention relates to a chemical synthesis preparation process, in particular to a preparation process for isopropyl antipyrine intermediate, an antipyretic and analgesic drug, isopropyl antipyrine. Background technique [0002] Isopropyl antipyrine has similar pharmacological effects to antipyrine and aminopyrine, and is suitable for the treatment of fever and mild to moderate pain. It is often used clinically for rheumatism, headache, toothache, migraine, etc. Neuralgia. [0003] Isopropyl antipyrine is widely used because of its small toxic and side effects and good curative effect. At present, there are more than 200 compound preparations containing isopropylantipyrine in the world, which are mainly used to treat pain, fever, cold, flu, muscle cramps, dysmenorrhea, migraine, etc., and have broad market prospects. [0004] The product has been included in the pharmacopoeias of Australia, Britain, Germany, France, Switzerland, Italy, Japan, Norw...

Claims

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Application Information

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IPC IPC(8): C07D231/22
Inventor 李兴泰王洪波陈梅
Owner SHANDONG XINHUA PHARMA
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