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A kind of method of reclaiming 3-isobutyl glutaric acid monoamide

A technology of isobutyl glutaric acid monoamide and isobutyl glutaric acid monoamide mother liquor, which is applied in the field of medicine and chemical industry, can solve problems such as the impact of environmental protection costs, achieve less pollution, reduce total organic carbon content, and increase atomic The effect of utilization

Active Publication Date: 2020-10-02
ZHEJIANG HUAHAI PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, compound 1 is resolved by a resolving agent to obtain compound 3 with a general yield of 33%~35%, and the yield of isomer 2 to obtain 1 through racemization is generally 40%~45%, that is to say, there is still 20% The above compound 1 directly forms solid waste and liquid waste without further treatment, which has a great impact on both environmental protection and cost

Method used

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  • A kind of method of reclaiming 3-isobutyl glutaric acid monoamide

Examples

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Effect test

preparation example

[0023] Preparation Example Ethyl Acetate Mother Liquor Example

[0024] Preparation of ethyl 3-isobutylglutaric acid monoamide acetate mother liquor: Weigh 500 g of the concentrated and dried racemate, add 2000 mL of toluene, heat up to 110-120 °C and stir, while separating water. After the water separation, cool down to 40-50°C, add 1500g of water and 500g of 30% NaOH aqueous solution dropwise, keep stirring for 3-4 hours after adding, cool down to 20-30°C, let stand to separate and separate the water phase, organic 1000.0g of water was added to the phase, stirred, and the layers were separated, and the water phase was separated and combined. Add concentrated hydrochloric acid dropwise to the water phase within the range of 0-10°C to adjust the pH to 1.5-4, and the adjustment is completed. Add 1000 and 600ml of ethyl acetate respectively, stir, let stand to separate layers, combine the organic phases, distill under reduced pressure to 800mL, slowly cool down to 0±5°C, filter...

example 1

[0026] Take the ethyl acetate mother liquor 750ml of suction filtration, weigh to obtain 155g after concentrating to dryness. Add 300g of water to the evaporated system, heat up to 40°C, add 100g of 30% liquid caustic soda to the system to adjust the pH to 14, cool down the pH-adjusted system to 20°C, and start adding concentrated hydrochloric acid dropwise until the pH is equal to 2. After adjusting the pH to 0°C, lower the temperature to 0°C, keep stirring for 3 hours, and filter and dry the filter cake. Add 350ml of toluene to the dried filter cake to make slurry for 1 hour, filter and dry with suction to obtain 75g of 3-isobutylglutaric acid monoamide, the yield is 15.0%, and the purity is 99.73%.

example 2

[0028] Take the ethyl acetate mother liquor 750ml of suction filtration, weigh to obtain 155g after concentrating to dryness. Add 200g of water to the evaporated system, raise the temperature to 45°C, add 100g of 30% liquid caustic soda to the system to adjust the pH to 14, cool down the pH-adjusted system to 30°C, and start adding concentrated hydrochloric acid dropwise until the pH is equal to 2. After adjusting the pH to 5°C, lower the temperature to 5°C, keep stirring for 2 hours, and filter and dry the filter cake. Add 300ml of toluene to the dried filter cake to make slurry for 2 hours, filter and dry with suction to obtain 78.3g of 3-isobutylglutaric acid monoamide, the yield is 15.6%, and the purity is 99.64%.

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Abstract

The invention discloses a method for recovering 3-carbamoymethyl-5-methylhexanoic acid from mother liquor containing more than 20% of pregabalin intermediate 3-carbamoymethyl-5-methylhexanoic acid. The method comprises steps as follows: a) concentrating the mother liquor to be dry and then adding water to the system; b) heating the system and adding liquid caustic soda to the system to adjust the pH; c) cooling the system and adding hydrochloric acid to the system to adjust the pH; d) continuously performing cooling, temperature holding, suction filtration and drying on the system with the pH adjusted; e) adding a solvent to a dried sample for pulping and performing suction filtration and drying to obtain the finished product. The method for recovering the 3-carbamoymethyl-5-methylhexanoic acid is environment-friendly, simple, convenient and little in pollution.

Description

technical field [0001] The invention provides a method for recovering 3-isobutylglutaric acid monoamide from the mother liquor of pregabalin intermediate, which belongs to the field of medicine and chemical industry. [0002] Background of the invention [0003] Pregabalin, English name Pregabalin, is a novel gamma-aminobutyric acid (GABA) receptor antagonist developed by Pfizer. Approved in June 2005 for the auxiliary treatment of partial-onset epilepsy in adults, it is the most promising drug among the epilepsy drugs that have been developed. The number of times is less, and it has the advantages of anti-anxiety effect and no drug-drug interaction with existing antiepileptic drugs, so it is convenient to be used in combination with other antiepileptic drugs to synergize the antiepileptic effect. In March 2006, the indication was added to treat generalized anxiety disorder and social anxiety disorder. In 2009, it was approved to treat spinal cord injury, trauma, multiple sc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C233/05C07C231/24
Inventor 刘幕松张靖东张文灵王鹏
Owner ZHEJIANG HUAHAI PHARMA CO LTD
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