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Dezocine production process

A technical process, the technology of dezocine, applied in the field of medicinal chemistry, can solve the problems of low reaction safety, harsh reaction conditions, long synthesis cycle, etc., and achieve the effect of improving the quality of finished products, shortening the synthesis cycle, and increasing the yield

Inactive Publication Date: 2019-09-27
JINAN LIMIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the deficiencies of the prior art, the present invention provides a dezocine production process, which solves the problems of many synthesis steps, cumbersome operation, long synthesis cycle, harsh reaction conditions in some parts, and low safety of individual reactions.

Method used

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Embodiment 1

[0048] Such as figure 2 As shown, the embodiment of the present invention provides the synthesis process of diazolamide salt comprising the following steps:

[0049] 1) Ruan's nickel process: First, add 78kg of purified water to the SF-100L reaction kettle with an opening, start stirring, slowly add 32.8kg of sodium hydroxide, stir and dissolve, then turn on the cooling device and cool down to 50°C , turn off the cooling device, add 7.87kg of 50% aluminum-nickel alloy in batches under stirring, then, after adding, stir for 10 minutes, turn on the heating device, raise the temperature to 97°C, keep stirring for 30 minutes, turn off the heating device, then turn on the cooling device, and cool down to 40°C, stop stirring, let it stand for 15 minutes, absorb the upper alkali water layer with vacuum, wash with purified water 3 times, 40kg each time, until the pH is 7.5, and finally put it in a stainless steel bucket, and finally, wash with absolute ethanol 2 times, 4L each time,...

Embodiment 2

[0053] Such as image 3 As shown, the embodiment of the present invention provides a synthesis process of methyl dezocine salt comprising the following steps:

[0054] 1) Primary dissociation: First, add 5.76kg of diazolamide salt, 28kg of purified water and 24kg of ethyl acetate into the SF-100L reactor, start stirring, add concentrated ammonia water dropwise until the pH value is 9.5, and stir for 15 minutes , then, turn off the stirring, let stand to separate the layers, separate the organic layer, extract the aqueous layer with ethyl acetate 3 times, 7.5L each time, combine the organic phases, and finally, wash the organic phase twice with purified water, 7.5L each time, The organic phase was concentrated under reduced pressure, and the solvent was evaporated to obtain an oily substance, that is, a primary free base;

[0055] 2) One-time splitting: First, add 2.91kg of L-tartaric acid and 37.4kg of anhydrous methanol into the SF-100L reactor, start stirring, after stirrin...

Embodiment 3

[0060] Such as Figure 4 As shown, the synthesis process of crude dezocine provided by the embodiment of the present invention includes the following steps:

[0061] 1) Demethylation process: In the SF-100L reactor, add 1.82kg of methyl dezocine salt and 16L of 48% hydrobromic acid, start stirring, pass in nitrogen protection, turn on the heating device, and wait until the reflux is stable. Reflux reaction for 2 hours, turn off the heating device, turn on the cooling device, then, when the temperature drops to about 80°C, turn off the cooling device, turn on the heating device and the water circulation vacuum system, evaporate the solvent to obtain a solid, filter it while it is hot, and use 400ml of purified water After washing, the filtrate was cooled to room temperature, placed in a freezer, cooled and crystallized for more than 4 hours, and finally, filtered to obtain dezocine hydrobromide solid;

[0062] 2) Alkalization process: first, in the SF-100L reactor, add dezocin...

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Abstract

The invention provides a dezocine production process, and relates to the technical field of medical chemistry. The dezocine production process comprises the following steps of 1) synthesis of dezocine ammonium salt, 2) synthesis of methyl dezocine salt, 3) synthesis of a crude dizocine product and 4) refining and packaging of the crude dizocine product. By means of the four processes of synthesis of dezocine ammonium salt, synthesis of methyl dezocine salt, synthesis of the crude dizocine product and refining and packaging of the crude dizocine product, the synthesis steps and the reaction conditions are optimized, the synthesis cycle is shortened, and meanwhile the detailed processes of the synthesis of dezocine ammonium salt, synthesis of methyl dezocine salt, synthesis of the crude dizocine product and refining of the crude dizocine product are described in details; key process parameters and product quality standards are defined, thus the dezocine production process can rapidly grasp key control points, and the synthesis reaction can be helped to be conducted efficiently and stably.

Description

technical field [0001] The invention relates to the technical field of medicinal chemistry, in particular to a dezocine production process. Background technique [0002] Dezocine (13-amino-5,6,7,8,9,10,11,12-octahydro-5-methyl-5,11-methylenebenzocyclodecen-3-ol) is White or off-white crystalline powder, odorless. This product is soluble in methanol, ethanol or glacial acetic acid, slightly soluble in acetone, ethyl acetate or chloroform, and almost insoluble in water. Dezocine is a powerful opioid analgesic. Dezocine can relieve postoperative pain, and its analgesic intensity, onset time and duration of action are comparable to morphine. When the steady-state plasma concentration exceeds 5-9ng / ml, it can relieve postoperative pain; when the average peak concentration reaches 45ng / ml, adverse reactions will occur. The time for the maximum analgesic effect is 20-60 minutes later than the peak blood concentration time. Due to the good tolerance and safety of dezocine, the ma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/10C07C213/02C07C215/64C07C213/08C07C217/74
CPCC07B2200/13C07C213/02C07C213/08C07C213/10C07C2603/80C07C215/64C07C217/74
Inventor 许祚芝赵先亮柴丽君
Owner JINAN LIMIN PHARMA
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