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
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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

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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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Example Embodiment

[0035] Example 1

[0036] The preparation method of L-aminopropanol of this embodiment includes the following steps:

[0037] 1) First dissolve 50g of L-alanine in 500ml of deionized water, and then mix it with 50g of sulfuric acid with a mass percentage of 85%;

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

[0039] 3) After the reaction, the filtrate is filtered and distilled under reduced pressure in a concentration tank. The water is evaporated off. The concentrated solution is cooled. After stirring, the insoluble substances are removed by filtration. The pure filtrate obtained is rectified in the rectifying tower and subjected to high vacuum. After rectification, L-aminopropanol with a purity of 99.5% was obtained, and the specific rotation reached +17.70°.

[0040] The filtered cake containing the ruthenium-carbon catalyst can be returned to step 2...

Example Embodiment

[0042] Example 2

[0043] The preparation method of L-aminopropanol of this embodiment includes the following steps:

[0044] 1) First dissolve 120g of L-alanine in 850ml of deionized water, and then mix with 100g of sulfuric acid with a mass percentage of 85%;

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

[0046] 3) After the reaction, the filtrate is filtered and distilled under reduced pressure in a concentration tank. The water is evaporated off. The concentrated solution is cooled. After stirring, the insoluble substances are removed by filtration. The pure filtrate obtained is rectified in the rectifying tower and subjected to high vacuum. After rectification, L-aminopropanol with a purity of 99.9% was obtained, and the specific rotation reached +17.8°.

[0047] The filtered cake containing the ruthenium-carbon catalyst can be returned to st...

Example Embodiment

[0048] Experimental 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 the effect of using nickel catalysts for hydrogenation reduction is not good, you can choose precious metal catalysts such as palladium, platinum, rhodium, etc.

[0050] Preparation of Ruthenium on Carbon Catalyst

[0051] Activated carbon supported nail catalysts are widely used as hydrogenation catalysts because of their good hydrogenation performance. The methods for preparing ruthenium-carbon catalyst 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 matrix in a certain solvent for a period of time, so that the matrix compound can be more uniformly adsorbed on the surface of the carrier, then filter or evaporate the solvent at a c...

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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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