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Method for recycling S-mandelic acid from atomoxetine hydrochloride production waste liquid

A technology of atomoxetine hydrochloride and mandelic acid, applied in organic chemical methods, separation/purification of carboxylic acid compounds, preparation of carboxylic acid salts, etc., can solve environmental pollution, waste of resources, no separation and purification and comprehensive utilization of recycling and other issues, to achieve the effect of stable process, easy control, and realization of circular economy

Active Publication Date: 2016-08-17
AMICOGEN CHINA BIOPHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The waste liquid of S-mandelic acid sodium salt solution produced in the production process of atomoxetine hydrochloride is mixed with other substances as waste liquid, without separation, purification, recycling and comprehensive utilization, which not only pollutes the environment, but also causes certain waste of resources

Method used

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  • Method for recycling S-mandelic acid from atomoxetine hydrochloride production waste liquid

Examples

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Effect test

Embodiment 1

[0032] (1) In a 1000mL three-neck flask, add 200mL of atomoxetine hydrochloride production waste liquid containing 10wt% S-mandelic acid; start stirring, add concentrated hydrochloric acid dropwise at 25°C, and adjust the pH of the system to be 3.0; then add 160mL of acetic acid Ethyl ester, stirred at 25°C for 30 minutes; stopped stirring, and stood still at 25°C for 20 minutes; separated, removed the lower aqueous phase, and kept the upper organic phase.

[0033] (2) Transfer the organic phase obtained in the previous step to a 500mL single-necked flask, carry out vacuum distillation at 35°C, recover the solvent, and precipitate a solid after evaporation to dryness to obtain 18.3g of S-mandelic acid crude product;

[0034] (3) Add 18.3g of crude S-mandelic acid and 146mL of mixed solvent (ethyl acetate:n-heptane=1:3) into a 500mL three-necked flask; start stirring, heat up to 65°C, stir for 20min to dissolve; slowly cool down and crystallize , cooling down to 5°C for about 5...

Embodiment 2

[0036] (1) In a 1000mL three-necked flask, add 300mL of atomoxetine hydrochloride production waste liquid containing 10wt% S-mandelic acid; start stirring, add concentrated sulfuric acid dropwise at 25°C, and adjust the pH of the system to be 2.5; then add 300mL of acetic acid Ethyl ester, stirred at 25°C for 30 minutes; stopped stirring, and stood still at 25°C for 20 minutes; separated, removed the lower aqueous phase, and kept the upper organic phase.

[0037] (2) Transfer the organic phase obtained in the previous step to a 1000mL single-necked flask, carry out vacuum distillation at 35°C, recover the solvent, and precipitate a solid after evaporation to dryness to obtain 26.8g of S-mandelic acid crude product;

[0038] (3) Add 26.8g of crude S-mandelic acid and 214mL of mixed solvent (ethyl acetate: n-heptane = 1:4) into a 500mL three-necked flask; start stirring, heat up to 70°C, stir for 20min to dissolve; slowly cool down and crystallize , cooling down to 5°C for about...

Embodiment 3

[0040] (1) In a 1000mL three-necked flask, add 300mL of atomoxetine hydrochloride production waste liquid containing 10wt% S-mandelic acid; start stirring, add phosphoric acid dropwise at 25°C, and adjust the pH of the system to be 2.0; then add 300mL of ethyl acetate For ester, stir at 25°C for 30min; stop stirring, and let stand at 25°C for 20min; separate the liquid, remove the lower aqueous phase, and keep the upper organic phase.

[0041] (2) Transfer the organic phase obtained in the previous step to a 1000mL single-necked flask, carry out vacuum distillation at 35°C, recover the solvent, and precipitate a solid after evaporation to dryness to obtain 26.4g of S-mandelic acid crude product;

[0042] (3) Add 26.4g of crude S-mandelic acid and 238mL of mixed solvent (ethyl acetate: n-heptane = 1:4) into a 500mL three-necked flask; start stirring, heat up to 70°C, stir for 20min to dissolve; slowly cool down and crystallize , cooling down to 5°C for about 5 hours; growing cr...

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Abstract

The invention relates to a method for recycling S-mandelic acid from atomoxetine hydrochloride production waste liquid, and belongs to the technical field of S-mandelic acid recycling. The method includes the steps that inorganic acid is added into atomoxetine hydrochloride production waste liquid to regulate the pH value of the system; then an organic solvent is added, and stirring, standing and skimming are carried out; an organic phase is subjected to reduced pressure distillation, and an S-mandelic acid crude product is separated out after drying by distillation; an organic solvent is added into the S-mandelic acid crude product, the temperature is increased to dissolution, the temperature is slowly decreased for crystallization, crystal growing, filtering, washing and drying are carried out, and an S-mandelic acid fine product is obtained. According to the method, the process is stable, reaction conditions are easy to control, no pollution is caused to the environment, cost is low, the recycling rate is high, and industrialization is easy to realize.

Description

technical field [0001] The invention relates to a method for recovering S-mandelic acid from atomoxetine hydrochloride production waste liquid, and belongs to the technical field of S-mandelic acid recovery. Background technique [0002] Atomoxetine hydrochloride is a chemical drug used in the treatment of ADHD in children and adolescents. Atomoxetine hydrochloride is the hydrochloride salt form of R-atomoxetine. The source of R-atomoxetine is the chiral resolution of racemic atomoxetine. The chiral resolution of racemic atomoxetine includes the following steps: racemic atomoxetine is first salted with S-mandelic acid (chiral resolving agent), and R-atomoxetine-S-mandelic Crystallization in the form of the acid salt was isolated. R-atomoxetine-S-mandelate is freed under alkaline conditions to obtain R-atomoxetine and waste liquid of S-mandelic acid sodium salt solution. R-atomoxetine reacts with HCl to generate atomoxetine hydrochloride. [0003] [0004] The waste l...

Claims

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Application Information

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IPC IPC(8): C07C59/50C07C51/02C07C51/48
CPCC07B2200/07C07C51/02C07C51/48C07C59/50
Inventor 方军张永志杜希兵王玲
Owner AMICOGEN CHINA BIOPHARM CO LTD
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