A kind of synthetic method of sodium phenytoin

A synthesis method and a technology of phenytoin sodium, applied in the field of biomedicine, can solve the problems of the impurity diphenylacetylene diurea being difficult to remove, long reaction time, many side reactions, etc., and achieve obvious competitive advantages, shorten the reaction time, and save a lot of costs. Effect

Active Publication Date: 2022-06-21
NINGBO POLYTECHNIC
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Problems solved by technology

[0007] In the existing method for synthesizing phenytoin sodium, the biggest problem is that the reaction time of the condensation process is too long, the side reactions are more, and the impurity toluene diurea is not easy to remove, resulting in low yield of phenytoin, low purity, and poor appearance crystal form , the color is deep, the post-treatment requires activated carbon decolorization, and even the crude phenytoin needs to be recrystallized and purified with ethanol solution, which further reduces the yield of phenytoin; in the process of salt formation, the precipitation of phenytoin sodium is difficult, the crystallization rate is slow, and the yield is low

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  • A kind of synthetic method of sodium phenytoin

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Effect test

Embodiment 1

[0032] Oxidation reaction: weigh 2.18g of benzoin, 5.4g of ferric trichloride hexahydrate, measure 13mL of glacial acetic acid, and 5.2mL of distilled water, pour them into a three-necked flask in turn, stir, and heat under reflux for 50min, and the reaction stops heating completely; The reaction solution was poured into a 100 mL beaker, 40 mL of distilled water was added, and an ice-salt bath was performed for 15 min. After the yellow needle-like crystals were precipitated, suction filtration was performed, and the filter cake was washed with distilled water for several times to obtain 2.14 g of bibenzoyl;

[0033] Condensation reaction: add 2.14g bibenzoyl, 1.80g urea, 2.13g potassium hydroxide, 0.06g 4-dimethylaminopyridine, 22mL n-butanol, 22mL distilled water to a 250mL three-necked round-bottom flask, stir magnetically at 115 The reaction was refluxed for 30 min, and the reaction was completely stopped heating; the reaction solution was cooled to room temperature, poured ...

Embodiment 2

[0036] Oxidation reaction: weigh 8.67g benzoin, 24.5g ferric trichloride hexahydrate, measure 50mL glacial acetic acid and 22mL distilled water, pour them into a three-necked flask in turn, start stirring, and heat under reflux for 52min, the reaction stops heating completely; after cooling, The reaction solution was poured into a 500 mL beaker, 173 mL of distilled water was added, and after an ice-salt bath for 16 min, yellow needle-like crystals were precipitated, suction filtered, and the filter cake was washed with distilled water for several times to obtain 8.5 g of bibenzoyl;

[0037] Condensation reaction: add 8.5g bibenzoyl, 7.4g urea, 9g potassium hydroxide, 0.26g 4-dimethylaminopyridine, 71mL n-butanol, 85mL distilled water to a 250mL three-necked round bottom flask, stir magnetically, heat at 118°C and reflux 35min, stop heating after the reaction is complete. The reaction solution was cooled to room temperature, poured into a 500 mL separatory funnel, extracted thr...

Embodiment 3

[0040] Oxidation reaction: weigh 10.71g of benzoin, 28g of ferric trichloride hexahydrate, weigh 64mL of glacial acetic acid, and 25mL of distilled water, pour them into a three-necked flask in turn, start stirring, and heat under reflux for 55min, the reaction is completely stopped heating; after cooling, the reaction The liquid was poured into a 500 mL beaker, 210 mL of distilled water was added, and after an ice-salt bath for 18 min, yellow needle-like crystals were precipitated, suction filtered, and the filter cake was washed with distilled water for several times to obtain bibenzoyl;

[0041] Condensation reaction: add 10.5g bibenzoyl, 9g urea, 10.64g potassium hydroxide, 0.305g 4-dimethylaminopyridine, 105mL n-butanol, 125mL distilled water to a 500mL three-necked round bottom flask, stir magnetically, heat to 119 The temperature was refluxed for 40 min, and the heating was stopped after the reaction was completed. The reaction solution was cooled to room temperature, p...

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Abstract

The invention relates to a method for synthesizing phenytoin sodium, which belongs to the technical field of biomedicine. The synthetic method of phenytoin sodium of the present invention comprises oxidation reaction, condensation reaction, salt-forming reaction, in condensation reaction, has promoted amidation reaction process by adding phase-transfer catalyst 4-dimethylaminopyridine; Adopt n-butanol and water two-phase system , greatly inhibited the generation of by-product diphenylacetylene diurea, and the reaction time was significantly shortened; in the salt-forming reaction, ethanol was used as a solvent, and after the reaction of sodium hydroxide ethanol solution and phenytoin, cyclohexane, a poor solvent, was added to promote the reaction of phenytoin Sodium is precipitated as white crystals. Compared with the salt-forming reaction in which water is used as a solvent, phenytoin sodium precipitates at a faster rate, with a higher degree of precipitation and higher purity.

Description

technical field [0001] The invention relates to a method for synthesizing phenytoin sodium, which belongs to the technical field of biomedicine. Background technique [0002] Phenytoin is the drug of choice for the treatment of epilepsy. It is clinically used for the treatment of grand mal epilepsy, psychomotor seizures and arrhythmia diseases. It can also be used for the treatment of trigeminal neuralgia, recessive dystrophic epidermolysis bullosa, epilepsy Chorea, episodic control disorder, myotonia, and cardiac conduction disorders in the event of overdose of tricyclic antidepressants. After more than half a century of clinical use, it has been proved to be one of the effective antiepileptic drugs, especially for grand mal epilepsy. [0003] At present, the synthesis method of phenytoin sodium mostly uses benzoin as raw material, and synthesizes phenytoin sodium through three steps of oxidation, condensation and salt formation, specifically: [0004] (1) benzoin oxidati...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D233/74
CPCC07D233/74
Inventor 史海波陈艳君蒋梦吉邵柯妹袁道远文志强
Owner NINGBO POLYTECHNIC
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