Aminobutanol resolution method

An aminobutanol, step-by-step technology, applied in the chemical field, can solve the problems of low resolution yield and low specific optical rotation of L-2-aminobutanol, and achieve the effect of high resolution yield and high optical rotation

Inactive Publication Date: 2017-10-13
嘉兴润博化工科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] But there are following problems in the resolution of DL-2-aminobutanol with tartaric acid as the resolving agent at present: the resolution yield is low, and the D-2-aminobutanol or L-2-aminobutanol ratio that resolution obtains low optical rotation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 1) Reaction: Assemble a three-necked reaction bottle in a water bath, add 79.9g of L-tartaric acid and 300ml of anhydrous methanol under stirring, heat to reflux at 65°C, add 23.7g of DL-2-aminobutanol dropwise; after the addition, Maintain the reaction temperature at 65°C, control the pH at 5.8-6.2, and react for 30 minutes to make DL-2-aminobutanol and L-tartaric acid react to generate D-2-aminobutanol-tartrate and L-2-aminobutanol-tartrate mixed solution;

[0021] 2) Precipitation of D-2-aminobutanol-tartrate: cool down the mixed solution in step 1) to 30°C, precipitate D-2-aminobutanol-tartrate and filtrate, filter and vacuum dry to obtain 23.5g D- 2-aminobutanol-tartrate, specific rotation﹦23.8;

[0022] 3) Precipitation of L-2-aminobutanol-tartrate: Put the filtrate in step 2) into an evaporator to evaporate, remove methanol, add 237ml of water to the evaporation residue, raise the temperature to 50°C and maintain it for 20 minutes to obtain The clarified filtra...

Embodiment 2

[0026] 1) Reaction: Assemble a three-necked reaction flask in a water bath, add 62.4g of L-tartaric acid and 300ml of anhydrous methanol under stirring, heat to reflux at 65°C, add 29.6g of DL-2-aminobutanol dropwise; after the addition, Maintain the reaction temperature at 55°C, control the pH at 6.2-6.5, and react for 30 minutes to make DL-2-aminobutanol and L-tartaric acid react to generate D-2-aminobutanol-tartrate and L-2-aminobutanol-tartrate mixed solution;

[0027] 2) Precipitation of D-2-aminobutanol-tartrate: cool down the mixed solution in step 1) to 25°C, precipitate D-2-aminobutanol-tartrate and filtrate, filter and dry in vacuum to obtain 29.5g D- 2-aminobutanol-tartrate, specific rotation﹦23.5;

[0028] 3) Precipitation of L-2-aminobutanol-tartrate: Put the filtrate in step 2) into an evaporator to evaporate, remove methanol, add 237ml of water to the evaporation residue, raise the temperature to 50°C and maintain it for 20 minutes to obtain The clarified filt...

Embodiment 3

[0032] 1) Reaction: Assemble a three-necked reaction bottle in a water bath, add 79.9g of L-tartaric acid and 300ml of anhydrous methanol under stirring, heat to reflux at 65°C, add 47.4g of DL-2-aminobutanol dropwise; after the addition, Maintain the reaction temperature at 60°C, control the pH at 6.5-7.0, and react for 30 minutes to make DL-2-aminobutanol and L-tartaric acid react to generate D-2-aminobutanol-tartrate and L-2-aminobutanol-tartrate mixed solution;

[0033] 2) Precipitation of D-2-aminobutanol-tartrate: cool down the mixed solution in step 1) to 28°C, precipitate D-2-aminobutanol-tartrate and filtrate, filter and vacuum dry to obtain 51.1g D- 2-aminobutanol-tartrate, specific rotation﹦23.2;

[0034] 3) Precipitation of L-2-aminobutanol-tartrate: Put the filtrate in step 2) into an evaporator to evaporate, remove methanol, add 237ml of water to the evaporation residue, raise the temperature to 55°C and maintain it for 20 minutes to obtain The clarified filtra...

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Abstract

The invention relates to an aminobutanol resolution method, which comprises: 1) carrying out a reaction: dissolving L-tartaric acid in anhydrous methanol, heating to a temperature of 65-55 DEG C, adding DL-2-aminobutanol to the L-tartaric acid methanol solution in a dropwise manner, carrying out a reaction, and controlling the pH value of the reaction system at 5-7; 2) precipitating D-2-aminobutanol-tartrate: cooling the mixing liquid obtained in the step 1) to a temperature of 35-25 DEG C to precipitate the D-2-aminobutanol-tartrate; 3) precipitating L-2-aminobutanol-tartrate: evaporating the filtrate in the step 2) to remove the methanol, adding water, controlling the temperature at 55-45 DEG C to obtain a clarified liquid, and cooling to a temperature of 15-5 DEG C so as to precipitate the L-2-aminobutanol-tartrate; and 4) preparing D-2-aminobutanol and L-2-aminobutanol: respectively adding an alkali liquid to the D-2-aminobutanol-tartrate precipitated in the step 2) and the L-2-aminobutanol-tartrate precipitated in the step 3), carrying out alkali precipitation, and respectively rectifying the filtrates so as to obtain the D-2-aminobutanol having the specific rotation of more than or equal to + / -10 and the L-2-aminobutanol having the specific rotation of more than or equal to + / -10.

Description

technical field [0001] The invention mainly belongs to the field of chemistry, and specifically refers to a method for splitting aminobutanol. Background technique [0002] Aminobutanol is a chiral amino alcohol, which has been widely used in the fields of medicine and chemical industry. It can be used as an important intermediate to produce active butanol derivatives, and can also be used to prepare emulsifiers, surfactants and vulcanization accelerators. The D-2-aminobutanol obtained through resolution can be used to synthesize the intermediate of the anti-tuberculosis drug ethambutol, and can also be used as a raw material for antibacterial agents and the like. [0003] The existing resolution of DL-2-aminobutanol usually adopts a chemical resolution method, and the chemical resolution method mostly uses tartaric acid as a resolving agent. [0004] But there are following problems in the resolution of DL-2-aminobutanol with tartaric acid as the resolving agent at presen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C215/08C07C213/10C07B57/00
CPCC07C215/08C07B57/00C07B2200/07C07C213/10
Inventor 倪平杨玉淳明虎
Owner 嘉兴润博化工科技有限公司
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