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A method for splitting dl-2-aminopropanol to prepare 1-2-aminopropanol

A technology for DL-2-, aminopropanol, applied in the field of splitting DL-2-aminopropanol to prepare L-2-aminopropanol, can solve the problems of high price of chiral raw materials and reducing agents, and achieve improved utilization. The effect of high yield and split yield

Inactive Publication Date: 2019-05-03
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chiral L-2-aminopropanol is generally prepared by reducing chiral 2-aminopropionic acid or its derivatives, and the chiral raw materials and reducing agents are relatively expensive
Most of the 2-aminopropanols obtained by general synthetic methods are racemates, and there is no economically feasible method for splitting racemic 2-aminopropanols to prepare L-2-aminopropanols

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] In a 1-liter flask, add 450 grams of ethanol and 37.5 grams (0.5 moles) of racemic DL-2-aminopropanol, stir at room temperature to dissolve and clarify, stir while cooling down, add dropwise 75 grams (0.5 moles) of L-tartaric acid and A clear solution of 150 grams of distilled water, the rate of addition is controlled so that the internal temperature does not exceed 50°C, and the temperature is lowered to 0-5°C after the addition. 3 grams of seed crystals (L-tartaric acid-L-2-aminopropanol seed crystals) were added, stirred slowly for 20 hours for crystallization, and a large amount of crystals were precipitated. Filter, wash the solid with a small amount of ethanol, and dry it under vacuum at 25°C to obtain 49.4 g of L-tartrate-L-2aminopropanol acid salt. The filtrate was spin-dried under reduced pressure to obtain 63 g of acid salt.

[0021] Disperse 49.4 grams (0.22 moles) of L-tartaric acid-L-2 aminopropanol acid salt in 200 milliliters of dehydrated alcohol, add 17...

Embodiment 2

[0023] In a 1000 ml flask, add 270 grams of methanol and 37.5 grams (0.5 moles) of racemic DL-2-aminopropanol, stir at room temperature to dissolve and clarify, stir while cooling down, add dropwise 75 grams (0.5 moles) of L-tartaric acid and A clear solution of 70 grams of distilled water, control the rate of dropping, so that the internal temperature does not exceed 40 ° C, after the addition, cool down to 0-5 ° C, add 3 grams of seed crystals, slowly stir and crystallize for 16 hours, and a large number of crystals are precipitated. After filtering, the filter cake was washed with a small amount of methanol, and dried under vacuum at 25°C to obtain 51.8 g of L-tartaric acid-L-2 aminopropanol acid salt, and the filtrate was spin-dried under reduced pressure to obtain 60 g of acid salt.

[0024] Disperse 51.8 grams (0.23 moles) of L-tartaric acid-L-2-aminopropanol acid salt in 150 milliliters of methanol, add 25.8 grams (0.46 moles) of potassium hydroxide at room temperature i...

Embodiment 3

[0026] In a 1000 ml flask, add 270 grams of isopropanol and 37.5 grams (0.5 moles) of racemic DL-2-aminopropanol, stir at room temperature to dissolve and clarify, stir while cooling down, add dropwise 75 grams (0.5 moles) of L-tartaric acid and a clear solution of 180 grams of distilled water, control the speed of dropping, so that the internal temperature does not exceed 50 ° C, after the addition, cool down to 0-5 ° C, add about 5 grams of seed crystals, slowly stir and crystallize for 24 hours, and a large number of crystals are precipitated. After filtering, the filter cake was washed with a small amount of isopropanol, and dried under vacuum at 25°C to obtain 42.2 g of L-tartrate-L-2aminopropanol acid salt, and the filtrate was spin-dried under reduced pressure to obtain 70 g of acid salt.

[0027] Disperse 42.2 grams (0.188 moles) of L-tartaric acid-L-2-aminopropanol acid salt obtained in 150 milliliters of isopropanol, add 13.1 grams (0.226 moles) of magnesium hydroxide...

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Abstract

The invention relates to a method for preparing L-2-aminopropanol by means of splitting DL-2-aminopropanol. The method includes steps of 1), dissolving L-tartaric acid in water to obtain L-tartaric acid aqueous solution; 2), dissolving the DL-2-aminopropanol in alcohol solvents at the room temperature, then stirring the DL-2-aminopropanol and the alcohol solvents under cooling conditions, simultaneously completely dropwise adding the L-tartaric acid aqueous solution into the DL-2-aminopropanol to obtain mixed solution, then cooling the mixed solution until the temperature of the mixed solution reaches 0-5 DEG C, and preserving heat to obtain cooled solution; 3), adding a small quantity of crystal seeds into the cooled solution, allowing the cooled solution to stand still at the temperatures ranging from -15 DEG C to +25 DEG C, crystallizing the cooled solution at the temperatures ranging from -15 DEG C to +25 DEG C for 16-24 hours and separating out L-tartaric acid-L-2-aminopropanol acid salt crystals; 4), dissolving the L-tartaric acid-L-2-aminopropanol acid salt crystals by the aid of alcohol solvents, adding inorganic bases into the L-tartaric acid-L-2-aminopropanol acid salt crystals in batches, stirring the inorganic bases and the L-tartaric acid-L-2-aminopropanol acid salt crystals until amino alcohol is completely free, carrying out suction filtration and carrying out reduced-pressure distillation on filter liquid to obtain the L-2-aminopropanol. The method has the advantages that processes are easy to implement, raw materials are high in utilization rate, and accordingly the method is suitable for large-scale production.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and relates to a method for preparing L-2-aminopropanol by splitting DL-2-aminopropanol. Background technique [0002] L-2-aminopropanol is an important organic chemical intermediate, one of the intermediates of the new generation of fluoroquinolone antibacterial drug levofloxacin and the pesticide dimethenamid, and an important organic Synthesis of chiral building blocks. Chiral L-2-aminopropanol is generally prepared by reducing chiral 2-aminopropionic acid or its derivatives, and the chiral raw materials and reducing agents are relatively expensive. Most of the 2-aminopropanols obtained by general synthesis methods are racemates, and there is no economically feasible method for splitting racemic 2-aminopropanols to prepare L-2-aminopropanols. Contents of the invention [0003] The technical problem to be solved by the present invention is to provide a method for splitting DL-2-amino...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C215/08C07C213/10
CPCC07B2200/07C07C213/10C07C215/08
Inventor 奚强吴忆雯王登马银刘裴卢洪宇舒畅
Owner WUHAN INSTITUTE OF TECHNOLOGY
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