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Aminohexenoic acid intermediate and preparation method thereof

A technology of vigabatrin and ethylene, applied in the field of medicine, can solve the problems of large discharge of post-treatment wastewater and solvent residues, etc.

Pending Publication Date: 2021-12-07
WUHAN WUYAO SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method still has many industrial technical difficulties to be solved
[0004] For example, 1,4-dichloro-2-butene reacts with diethyl malonate under alkaline conditions to prepare 2-vinylcyclopropane-1,1-diethyl dicarboxylate, and the yield needs to be improved , the discharge of post-treatment wastewater is large, and the prepared 2-vinylcyclopropane-1,1-diethyldicarboxylate has many problems such as solvent residues

Method used

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  • Aminohexenoic acid intermediate and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] 1) Reaction steps: Add 81.6Kg of 20% sodium ethoxide ethanol solution into the enamel reaction kettle, start stirring, and heat up to 55°C; weigh 40.3Kg of diethyl malonate, and add it dropwise to the above-mentioned enamel reaction kettle; Take 30Kg of trans-1,4-dichloro-2-butene and add it dropwise to the above-mentioned enamel reaction kettle, and the dropwise addition is completed in 1.5 to 2 hours; weigh 81.6Kg of 20% sodium ethylate ethanol solution, add it to the above-mentioned enamel In the reaction kettle, the dropwise addition is completed in 1 to 1.5 hours; the temperature is raised to 60°C, and the reaction is performed for 4.5 hours;

[0055] 2) Post-treatment: After the reaction is over, stop heating and cool down to 20°C; filter, transfer the mother liquor into an enamel reaction kettle, add 70g of hydroquinone, and reduce Concentrate under reduced pressure to obtain an oily substance, namely 2-vinylcyclopropane-1,1-diethyldicarboxylate. The yield was 9...

Embodiment 2

[0057] 1) Reaction steps: Add 72.6Kg of 20% sodium ethoxide ethanol solution into the enamel reaction kettle, start stirring, and heat up to 55°C; weigh 42.3Kg of diethyl malonate, and add it dropwise to the above-mentioned enamel reaction kettle; Take 30Kg of trans-1,4-dichloro-2-butene and add it dropwise to the above-mentioned enamel reaction kettle, and the dropwise addition is completed in 1.5 to 2 hours; weigh 90.6Kg of 20% sodium ethoxide ethanol solution, add it to the above-mentioned enamel In the reaction kettle, the dropwise addition is completed in 1 to 1.5 hours; the temperature is controlled at 55°C, and the reaction is 6 hours;

[0058] 2) Post-treatment: After the reaction is over, stop heating and cool down to 20°C; filter, transfer the mother liquor into an enamel reactor, add 70g of hydroquinone, and reduce the temperature at 55°C with a vacuum of not less than 0.07Mpa Concentrate under reduced pressure to obtain an oily substance, namely 2-vinylcyclopropane...

Embodiment 3

[0060] 1) Reaction steps: Add 97.9Kg of 20% sodium ethoxide ethanol solution into the enamel reaction kettle, start stirring, and heat up to 55°C; weigh 42.3Kg of diethyl malonate, and add it dropwise to the above-mentioned enamel reaction kettle; Take 30Kg of trans-1,4-dichloro-2-butene and add it dropwise to the above-mentioned enamel reaction kettle, and the dropwise addition is completed in 1.5 to 2 hours; weigh 65.3Kg of 20% sodium ethoxide ethanol solution, and add it to the above-mentioned enamel reaction kettle In the reaction kettle, the dropwise addition is completed in 1 to 1.5 hours; the temperature is raised to 65°C, and the reaction is carried out for 3 hours;

[0061] 2) Post-processing: After the reaction is over, stop heating and cool down to 20°C; filter, transfer the mother liquor into an enamel reaction kettle, add 70g of hydroquinone, and depressurize at 65°C with a vacuum degree of not less than 0.07Mpa Concentration gave an oily substance, namely 2-vinyl...

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Abstract

The invention provides an aminohexenoic acid intermediate 2-vinyl cyclopropane-1, 1-diethyl dicarboxylate and a preparation method thereof, application of the aminohexenoic acid intermediate 2-vinyl cyclopropane-1, 1-diethyl dicarboxylate in preparation of aminohexenoic acid, an aminohexenoic acid product and a preparation method thereof. The preparation method of the 2-vinyl cyclopropane-1, 1-diethyl dicarboxylate comprises the steps: (1) reacting 1, 4-dichloro-2-butene with diethyl malonate in a sodium ethoxide solution to obtain a reaction solution containing 2-vinyl cyclopropane-1, 1-diethyl dicarboxylate; and (2) carrying out purification treatment on the reaction solution, wherein the purification treatment comprises the steps: directly cooling and filtering the reaction solution, and collecting a filtrate containing 2-vinyl cyclopropane-1, 1-diethyl dicarboxylate. The 2-vinyl cyclopropane-1, 1-diethyl dicarboxylate prepared by the preparation method is high in yield, high in purity, few in solvent residue and raw material residue, simple, convenient and rapid to operate, free of wastewater discharge and suitable for large-scale production.

Description

technical field [0001] The present invention relates to the field of medicine. Specifically, the present invention relates to a vigabatrin intermediate and a preparation method thereof. Background technique [0002] The chemical name of Vigabatrin is 4-amino-5-hexenoic acid, and its molecular formula is C 6 h 11 NO 2 , with a molecular weight of 129.157, is an analogue of γ-aminobutyric acid (GABA), which can specifically bind to GABA aminotransferase and is irreversible, leading to an increase in the concentration of GABA in the brain, thereby exerting an antiepileptic effect. Vigabatrin can be used as an adjuvant therapy in patients who do not respond to other antiepileptic drugs, especially in patients with partial seizures (mainly for the control of complex partial seizures), and in West syndrome (infantile spasms) in babies. As an adjuvant drug, vigabatrin can obtain better curative effect. When used alone, it is effective in the treatment of newly diagnosed patie...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/343C07C69/743C07C227/04C07C67/56C07C229/30
CPCC07C67/343C07C69/743C07C227/04C07C67/56C07C229/30C07C2601/02
Inventor 朱毅张锐田俊锋王剑侠李雷
Owner WUHAN WUYAO SCI & TECH
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