Succinylcholine chloride preparation method

A technology of succinylcholine chloride and choline chloride is applied in the preparation of organic compounds, chemical instruments and methods, preparation of aminohydroxy compounds, etc., and can solve problems such as inflammable, explosive, highly toxic, and inconvenient to handle.

Inactive Publication Date: 2020-02-11
SHANGHAI XUDONG HAIPU PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process avoids the generation of acid gas, and the reaction equipment is simple, but it has the disadvantages of long reaction time and the use of flammable and explosive methyl chloride gas.
[0006] In the existing succinylcholine chloride synthesis process, there are disadvantages such as inconvenient post-processing of the product, low yield, exhaust gas or not environmentally friendly or highly toxic or flammable and explosive, and long reaction time.

Method used

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  • Succinylcholine chloride preparation method
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  • Succinylcholine chloride preparation method

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preparation example Construction

[0035] The preparation method of the present invention may include the following steps:

[0036] (1) Under solvent-free conditions, succinic acid and phosphorus pentachloride are reacted to form a mixture containing succinyl chloride; the mixture containing succinyl chloride is distilled under reduced pressure to collect succinyl chloride;

[0037] (2) Under anhydrous conditions, add dropwise or batchwise the succinyl chloride obtained in step (1) to the mixture of choline chloride and alcohol-free chloroform, and then react to form a mixture containing succinyl chloride The mixture containing succinylcholine chloride is neutralized, dissolved and precipitated to obtain succinylcholine chloride.

[0038] Preferably, the succinyl chloride is added dropwise, and the temperature range of the reaction liquid during dropwise addition is 50-60°C.

[0039] The preparation method of the present invention may also include the following steps:

[0040] (1-1) After reacting succinic acid and phos...

Embodiment 1

[0057] Put the stir bar in the reaction flask (1L) connected with the condenser, drying device, and lye absorption device, and add PCl in batches (3 times) 5 (277.7g×3,833.0g, 4.0mol), succinic acid (78.7g×3,236.2g, 2.0mol). Mix the reactants in the first batch with a glass rod and react at room temperature. After the reactants are basically liquefied and no obvious gas is generated, put in the second batch of PCl 5 React with succinic acid at room temperature. After the reaction solution has no obvious gas generation, put in the third batch of PCl 5 React with succinic acid at room temperature. After the reaction solution has no obvious gas generation, it is heated to 60°C for 1 hour. Collect POCl separately by vacuum distillation 3 And succinyl chloride (water pump decompression, oil bath heating temperature 60-80℃, fraction temperature 32-36℃, collect by-product POCl 3 , 556g, yield 90.7%; oil bath heating temperature 120-125℃, fraction temperature 36-97℃, collect POCl 3 And s...

Embodiment 2

[0062] Pour PCl into the reactor (20L) connected with condenser, stirrer, and lye absorption device in batches (3 times) 5 (5.29kg×3, 15.87kg, 76.21mol), succinic acid (1.50kg×3, 4.50kg, 38.11mol). Mix the reactants in the first batch with a stirrer, and react at room temperature. After the reactants are basically liquefied and no obvious gas is generated, put in the second batch of PCl 5 React with succinic acid at room temperature. After the reactant liquid has no obvious gas generation, put in the third batch of PCl 5 And succinic acid. React at room temperature. After the reaction solution has no obvious gas generation, it is heated to 60°C and stirred for 1 hour. Collect POCl separately by vacuum distillation 3 And succinyl chloride (water pump decompression, oil bath heating temperature 80-100℃, fraction temperature 40-76℃, collect by-product POCl 3 , 11.09kg, yield 94.9%; oil bath heating temperature 100-140℃, distillate temperature 76-95℃, collect POCl 3 And succinyl chl...

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Abstract

The invention relates to a succinylcholine chloride preparation method, and specifically discloses a synthetic method for preparing succinylcholine chloride by using succinic acid as a starting raw material through a chlorination reaction and an esterification reaction. According to the invention, the method has advantages of safe production, low production cost, high reaction efficiency and simple product purification, and is suitable for mass production of bulk drugs.

Description

Technical field [0001] The invention belongs to the field of drug synthesis, and specifically relates to a preparation method of succinylcholine chloride. Background technique [0002] Suxamethonium Chloride, also known as Scoline, is a white or off-white crystalline powder; it is odorless and has a salty taste; it is easily soluble in water, slightly soluble in ethanol or chloroform, and insoluble in ether; The melting point is 157-163°C. Its chemical name is 2,2-[(1,4-dioxo-1,4-butylene dichloride)bis(oxy)]bis[N,N,N-trimethylethylammonium] dihydrate , The molecular formula is C 14 H 30 Cl 2 N 2 O 4 ·2H 2 O, molecular weight is 397.34, structural formula is as follows: [0003] [0004] Succinylcholine chloride is a depolarizing neuromuscular blocker and can interact with the motor endplate N 2 Choline receptors bind to depolarize the endplate membrane and adjacent muscle cell membranes, block the transmission of nerve impulses at the neuromuscular junction, and cause skeletal m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C219/06C07C213/06C07C51/60C07C55/36
CPCC07C213/06C07C51/60C07C55/36C07C219/06
Inventor 谭昌恒姜坤张士俊陆翔宓柏权
Owner SHANGHAI XUDONG HAIPU PHARMA
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