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Synthetic method of L-aminopropanol

A technology of aminopropanol and synthetic method, which is applied in the preparation of aminohydroxyl compounds, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of prolonging the production cycle, flammability, increasing reaction steps, etc., and achieve emission reduction of SOD and SO2, the effect of reducing production cost and shortening the reaction steps

Inactive Publication Date: 2010-02-17
浙江凯迪药业有限公司
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0011] In the above two reduction methods for synthesizing L-aminopropanol, although the reaction conditions are all relatively mild, the NaBH used in the reduction method 4 , LiAlH 4 The reducing agent is expensive, flammable, dangerous, and highly toxic, and the product separation and purification procedures are complicated, which is not conducive to industrial production. A large amount of organic solvents are used in the synthesis and separation process, and solvent recovery is difficult in the production process. There are a lot of pollutants, such as waste water, waste gas, solid waste, etc., which are not conducive to environmental protection
[0012] In addition, the esterification reduction method needs to undergo an esterification reaction and then reduction to obtain the target product, which undoubtedly increases the reaction steps, prolongs the production cycle, and increases the production cost, which limits the application of this synthesis method in industrial production.

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  • Synthetic method of L-aminopropanol
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  • Synthetic method of L-aminopropanol

Examples

Experimental program
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Effect test

Embodiment 1

[0036] A kind of preparation method of L-aminopropanol of the present embodiment, it comprises the steps:

[0037] 1) Dissolve 50gL-alanine in 500ml of deionized water, then mix it with 50g of 85% sulfuric acid by mass;

[0038] 2) Add 250g of ruthenium carbon catalyst and pass in 5.6g (2.8mol) of hydrogen, control the reaction temperature at 88±2°C, pressurize at 8MPa, and stir at 500 rpm for 6 hours;

[0039] 3) After the reaction is finished, filter the filtrate, distill it under reduced pressure in a concentrated kettle, distill off the water, cool the concentrated solution, and filter to remove the insoluble substances therein after stirring evenly, and the obtained pure filtrate is rectified in a rectification tower, and then purified by high vacuum After rectification, L-aminopropanol with a purity of 99.5% is obtained, and the specific rotation reaches +17.70°.

[0040] Filter the filter cake of the ruthenium-containing carbon catalyst of gained, can return to step 2)...

Embodiment 2

[0043] A kind of preparation method of L-aminopropanol of the present embodiment, it comprises the steps:

[0044] 1) first dissolve 120gL-alanine in 850ml of deionized water, then mix it with 100g of 85% sulfuric acid by mass;

[0045] 2) Add 576g of ruthenium carbon catalyst and feed 12.32g (6.16mol) of hydrogen gas, control the reaction temperature to 82±2°C, pressurize at 9MPa, and stir at 600 rpm for 5 hours;

[0046]3) After the reaction is finished, filter the filtrate, distill it under reduced pressure in a concentrated kettle, distill off the water, cool the concentrated solution, and filter to remove the insoluble substances therein after stirring evenly, and the obtained pure filtrate is rectified in a rectification tower, and then purified by high vacuum After rectification, L-aminopropanol with a purity of 99.9% is obtained, and the specific rotation reaches +17.8°.

[0047] Filter the filter cake of the ruthenium-containing carbon catalyst of gained, can return ...

experiment example 1

[0049] The quality of the catalyst directly affects the effect of the hydrogenation reduction reaction, and the hydrogenation reaction mostly uses Pd / C, Pt / C, etc. as catalysts. When nickel catalyst is not effective for hydrogenation reduction, noble metal catalyst palladium, platinum, rhodium, etc. can be selected.

[0050] Preparation of Ruthenium Carbon Catalyst

[0051] Activated carbon-supported nail catalysts are widely used as catalysts for hydrogenation reactions due to their good hydrogenation performance. The methods for preparing ruthenium carbon catalysts include impregnation method, ion exchange method and liquid phase reduction method.

[0052] (a) Impregnation method The impregnation method is mainly to immerse the activated carbon and the parent in a certain solvent for a period of time, so that the parent compound can be more evenly adsorbed on the surface of the carrier, and then filter or evaporate the solvent at a certain temperature, dry, and then use Hi...

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Abstract

The invention provides a preparation method of L-aminopropanol, using L-alanine and H2 as main raw materials and carbon ruthenium as a catalyst to carry out direct catalytic hydrogenation to synthesize the L-aminopropanol. The method increases the selectivity of process reaction, accelerates reaction speed and shortens reaction step, thereby greatly reducing the production cost, increasing the L-aminopropanol yield, reducing the production of harmful wastes and realizing the greenization of the reaction process; and the aspects of energy saving and emission reduction of SOD and SO2 are obviously improved in order to realize less environment pollution. Any organic solvent is not added to the whole reaction process, thereby reducing the emission of pollutants, and protecting environment.

Description

technical field [0001] The invention relates to a preparation method of fine chemicals, in particular to a preparation method of a pharmaceutical intermediate, in particular to a synthesis method of L-aminopropanol. Background technique [0002] L-aminopropanol is the key intermediate for the synthesis of levofloxacin, and levofloxacin (levofxcain, DR-3355) is the S-shaped levorotatory optical isomer of ofloxacin ofloxacin, and its antibacterial activity is the latter. Twice as much as that of quinolones, with less toxic and side effects and high water solubility, it is one of the excellent broad-spectrum antibacterial drugs among quinolones. The antibacterial activity of levofloxacin is 8-128 times that of the enantiomer, and the effective rate against intestinal infection and gonococcal infection is 100%. It is one of the bulk drugs currently used clinically. The product was first successfully developed by Japan's Daiichi Pharmaceutical Co., Ltd. in the early 1990s. It of...

Claims

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Application Information

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IPC IPC(8): C07C215/08C07C213/00
Inventor 周秋火
Owner 浙江凯迪药业有限公司
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