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Nalmefene hydrochloride preparation method

A technology of nalmefene hydrochloride and naltrexone, which is applied in the field of preparation of nalmefene hydrochloride, can solve the problems of reducing drug safety, unsuitable waste liquid treatment, cumbersome steps, etc., to meet the needs of large-scale production and shorten the production cycle , The effect of simple process operation

Inactive Publication Date: 2015-04-15
ANHUI YOUCARE KAIYUE PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Now in the synthesis process of nalmefene hydrochloride, ammonium chloride solution is often used when terminating the reaction, but this will introduce ammonium salt impurities, the waste liquid is not suitable for disposal, and the safety of the drug is reduced, and many original steps are relatively cumbersome , which increases the cost of preparing

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment Construction

[0025] The preparation of nalmefene hydrochloride crude product:

[0026] Stir mechanically, add 153mL tetrahydrofuran, 11g triphenylphosphine bromide, and slowly add 34.5g potassium tert-butoxide in batches to a 1L dry and clean three-necked round-bottom flask under nitrogen protection. After stirring for 30±5min, add 17g of naltrexone in tetrahydrofuran solution (dissolved in 51ml of tetrahydrofuran) dropwise, and complete the dropwise addition after 4±0.5h, keep the temperature at 40±5°C, continue stirring for 9±1h, and monitor the end point of the reaction by high performance liquid phase .

[0027] After the reaction, control the temperature at 45±5°C, add 8.5mL of purified water dropwise, and complete the dropwise addition after 30±5min, keep the temperature and continue to stir for 10min. The solution was vacuum filtered with a 50mm Buchner funnel, the filter cake was washed with 21ml of tetrahydrofuran, and the filter cake was discarded. The filtrate was distilled und...

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PUM

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Abstract

The invention relates to a nalmefene hydrochloride preparation method, nalmefene hydrochloride preparation process is improved, the new process is easier to operate and easier to control, the production cycle is shortened, and the environment pollution is reduced, so that the new technology is more safe and reliable to meet the requirement of large scale production.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a preparation method of nalmefene hydrochloride. Background technique [0002] Nalmefene hydrochloride is indicated for the complete or partial reversal of opioid effects, including respiratory depression caused by natural or synthetic opioids. It is mainly used for emergency awakening of known or suspected opioid drug overdose or poisoning, acute brain and spinal cord injury, cerebral ischemia, cerebral infarction and other neurological damage diseases. Coma, shock and postoperative anesthesia awakening, alcoholism, anti-relapse treatment after detoxification, etc. [0003] Now in the synthesis process of nalmefene hydrochloride, ammonium chloride solution is often used when terminating the reaction, but this will introduce ammonium salt impurities, the waste liquid is not suitable for disposal, and the safety of the drug is reduced, and many original steps are rel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D489/08
CPCC07D489/08
Inventor 周如国
Owner ANHUI YOUCARE KAIYUE PHARMA
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