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Post-treatment method of N-amino-3-aza-bicyclo-[3.3.0] octane hydrochloride

A technology of octane hydrochloride and azabicycle is applied in the field of efficient post-processing of N-amino-3-azabicyclo[3.3.0]octane hydrochloride, and can solve the problems of unfriendly environment, cumbersome process, problems such as low production efficiency, to achieve the effects of environmental friendliness, simple process and low cost

Active Publication Date: 2014-06-04
HAISO TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above post-processing process is cumbersome, low production efficiency, high energy consumption, low yield, unguaranteed product quality, multiple use of different organic solvents, reduced safety, and unfriendly environment

Method used

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  • Post-treatment method of N-amino-3-aza-bicyclo-[3.3.0] octane hydrochloride

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] In a 5,000-liter reactor, 2,200 kilograms of materials to be treated containing N-amino-3-azabicyclo[3.3.0]octane hydrochloride were quantitatively detected and analyzed by gas chromatography containing N-amino-3-azabicyclo [3.3.0] 320 kg of octane, at 25°C, add industrial liquid caustic soda (sodium hydroxide solution) to the liquid to be treated to free the product, and then test by titration to make the concentration of sodium hydroxide reach 15%.

[0023] Put 0.1-0.6MPa steam into the jacket of the reaction kettle, and when fractions begin to appear, inject saturated water vapor into the bottom of the liquid to be treated, control the steam pressure at 0.1-0.6MPa, start steam distillation, collect fractions, and distill During the process, samples were continuously taken from the bottom of the pot, and monitored by gas chromatography (GC) or high performance liquid chromatography (HPLC) until the distillation was completed, and the resulting aqueous fraction containi...

Embodiment 2

[0026] Carry out the experiment with the method identical with embodiment 1, difference is to change the alkali metal hydroxide kind that the material to be treated adds, add respectively solid sodium hydroxide, solid potassium hydroxide to carry out experiment, experimental result is shown in Table 1.

[0027] Table 1

[0028] Alkali metal hydroxide

[0029] The results in Table 1 show that using solid sodium hydroxide or potassium hydroxide as a regulator can achieve high product yield and good quality.

Embodiment 3

[0031] Carry out experiment with the method identical with embodiment 1, difference is to change adding sodium hydroxide solution (industrial liquid caustic soda) to add solid sodium hydroxide, and change add-on. The mass percent concentration of alkali metal hydroxide in the adjusted material was 5%, 25%, 35%, and 50% to carry out the experiment, and the experimental results are shown in Table 2.

[0032] Table 2

[0033] Sodium hydroxide concentration%

[0034] It can be seen from Table 2 that during the steam distillation process, it is the water vapor that takes the product out of the distillation system for collection. In the process of steam distillation, the water in the system is constantly decreasing, and when the concentration of hydroxide is low, the water content in it is high, and the large amount of water in the distillation system can more fully carry out the steam distillation of the product, so sodium hydroxide The yield is relatively high when the ...

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Abstract

The invention provides a post-treatment method of N-amino-3-aza-bicyclo-[3.3.0] octane hydrochloride. The method is characterized by comprising the following steps: adjusting the acid-base property of N-amino-3-aza-bicyclo-[3.3.0] octane materials existing in different forms by alkali metal hydroxides, so that the product is free; then extracting and separating by adopting a steam distillation method; collecting a water solution fraction, adjusting the acid-base property of the fraction by a hydrochloric acid, so as to form hydrochloride; obtaining a powder product in a spray drying manner. By adopting the method disclosed by the invention, industrial production is achieved, the method has great application prospect, the yield of the obtained product is 95.4%, the content is 99.3% (nonaqueous titration), and the drying shrinkage is 0.3%. The product is even white solid powder, and is simple in process, environment-friendly, high in yield, low in cost and applicable to large-scale production.

Description

technical field [0001] The invention relates to an efficient aftertreatment method of N-amino-3-azabicyclo[3.3.0]octane hydrochloride. Background technique [0002] N-Amino-3-azabicyclo[3.3.0]octane hydrochloride is an important intermediate of gliclazide, which is a second-generation sulfonylurea oral hypoglycemic drug with hypoglycemic and The dual effect of improving blood coagulation function is a hypoglycemic drug widely used all over the world, including my country. [0003] At present, in the reports of the post-treatment method and process of N-amino-3-azabicyclo[3.3.0]octane hydrochloride at home and abroad, the post-treatment method is cumbersome, requires organic solvents, low yield, and unfriendly environment. . The post-processing method of patent CN101235011A is: extract with toluene, then acidify with hydrochloric acid to form a salt, distill to remove toluene and a small amount of water, obtain the product hydrochloride solid, filter and separate, and recrys...

Claims

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Application Information

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IPC IPC(8): C07D209/52
CPCC07D209/52
Inventor 邓嘉伦刘小成李翔余丹刘昱蔡光威李自勇
Owner HAISO TECH
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