Synthesis method of 4-tert-butyl cyclohexyl acetic acid

A synthesis method and technology of tert-butylbenzene are applied in the field of synthesis of pharmaceutical intermediates, and can solve the problems such as inability of reaction, large phosphorus-containing waste water, high environmental protection pressure, etc., and achieve easy satisfaction of equipment conditions, low production cost, and reaction steps. short effect

Inactive Publication Date: 2022-04-05
江苏云朴医药新材料科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] This method obtains 4-tert-butylcyclohexanoic acid through four-step reaction, and the main defect that this method exists is: produce a large amount of phosphorus-containing waste water in the reaction process, environmental protection pressure is bi...

Method used

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  • Synthesis method of 4-tert-butyl cyclohexyl acetic acid
  • Synthesis method of 4-tert-butyl cyclohexyl acetic acid
  • Synthesis method of 4-tert-butyl cyclohexyl acetic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Dissolve 50.00g (0.26mol) of 4-tert-butylphenylacetic acid in 250ml of methanol, add the solution to the hydrogenation kettle, add 5.00g of palladium-carbon catalyst to the solution, close the cover, ensure that it is firmly fixed, and then replace it with 0.3MPa nitrogen in turn 3 times, 0.3MPa hydrogen replacement 2 times, after the replacement, fill the kettle with 6MPa hydrogen and start stirring. Observe the change of the pressure gauge during the process. When the pressure in the kettle is lower than 4MPa, hydrogen is added to 6MPa, and the pressure in the straight kettle is basically stable. After the pressure in the kettle is stabilized, stop stirring, let it stand for 10 minutes, open the exhaust valve to empty the pressure in the kettle, replace it with 0.3MPa nitrogen twice, then empty the pressure in the kettle, open the lid of the kettle to mix and filter the kettle, and the obtained filtrate Concentrate by vacuum precipitation to about 100ml.

[0040] Slo...

Embodiment 2

[0042] Dissolve 50.00g (0.26mol) of 4-tert-butylphenylacetic acid in 250ml of methanol, add the solution to the hydrogenation kettle, add 15.00g of Raney nickel to the solution, close the cover, ensure that it is firmly fixed, and then replace it with 0.3MPa nitrogen in turn 3 times, 0.3MPa hydrogen replacement 2 times, after the replacement, fill the kettle with 6MPa hydrogen and start stirring. Observe the change of the pressure gauge during the process. When the pressure in the kettle is lower than 4MPa, hydrogen is added to 6MPa, and the pressure in the straight kettle is basically stable. After the pressure in the kettle is stabilized, stop stirring, let it stand for 10 minutes, open the exhaust valve to empty the pressure in the kettle, replace it with 0.3MPa nitrogen twice, then empty the pressure in the kettle, open the lid of the kettle to mix and filter the kettle, and the obtained filtrate Concentrate by vacuum precipitation to about 100ml.

[0043] Slowly pour the...

Embodiment 3

[0046] Dissolve 50.00g (0.26mol) of 4-tert-butylphenylacetic acid in 250ml of ethanol, add the solution to the hydrogenation kettle, add 15.00g of Raney nickel to the solution, close the cover, ensure that it is firmly fixed, and then replace it with 0.3MPa nitrogen in turn 3 times, 0.3MPa hydrogen replacement 2 times, after the replacement, fill the kettle with 6MPa hydrogen and start stirring. Observe the change of the pressure gauge during the process. When the pressure in the kettle is lower than 4MPa, hydrogen is added to 6MPa, and the pressure in the straight kettle is basically stable. After the pressure in the kettle is stabilized, stop stirring, let it stand for 10 minutes, open the exhaust valve to empty the pressure in the kettle, replace it with 0.3MPa nitrogen twice, then empty the pressure in the kettle, open the lid of the kettle to mix and filter the kettle, and the obtained filtrate Concentrate by vacuum precipitation to about 100ml.

[0047] Slowly pour the ...

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Abstract

The invention discloses a synthesis method of 4-tert-butyl cyclohexyl acetic acid, which comprises the following steps: dissolving 4-tert-butyl phenylacetic acid in a solvent, adding a catalyst into the solvent, carrying out high-pressure catalytic hydrogenation reaction, after the reaction is finished, filtering out the catalyst from reaction liquid, desolventizing and concentrating, adding concentrated liquid into water to separate out solid, centrifuging, and drying to obtain the 4-tert-butyl cyclohexyl acetic acid. The refined 4-tert-butyl cyclohexyl acetic acid is obtained. According to the synthesis method provided by the invention, 4-tert-butylphenylacetic acid is adopted as a raw material, the raw material is cheap and easy to obtain, a target product can be obtained through a one-step catalytic hydrogenation reaction, the synthesis process is efficient and simple, the reaction steps are short, the production cost is relatively low, the product yield is high, the product purity is high, and ions harmful to subsequent coupling reaction are not contained; the method has obvious advantages on subsequent synthesis of buparvaquone. In the whole production process, reaction conditions are mild, safe and environment-friendly, equipment conditions are easy to meet, and industrial production is facilitated.

Description

technical field [0001] The invention relates to the technical field of synthesis of pharmaceutical intermediates, in particular to a synthesis method of 4-tert-butylcyclohexylacetic acid. Background technique [0002] Theilerisis is a general term for diseases caused by various scorch worms of the genus Theileketaylus parasitizing cattle, sheep and other wild animals, among which bovine annulus is the most common. Bovine theileriasis is a bovine blood protozoan disease caused by Theileria annulus, which has the characteristics of wide prevalence, high morbidity and mortality. After the pathogen is transmitted to cattle by ticks, it parasitizes in macrophages, lymphocytes, and red blood cells, and then causes a disease characterized by high fever, anemia, emaciation, and swelling of lymph nodes on the body surface, which in turn leads to the death of cattle. [0003] Bupavaquinone is currently a very effective drug for the treatment of bovine theilesisis. It competitively in...

Claims

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Application Information

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IPC IPC(8): C07C51/36C07C53/134
CPCC07C51/36C07C53/134Y02P20/584
Inventor 杨浩浩康兵权张振兴杨小侠
Owner 江苏云朴医药新材料科技有限公司
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