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Chiral resolution method of methyl 2-(6-hydroxy-2, 3-dihydrobenzofuran-3-yl)acetate

A technology of methyl acetate and chiral separation, which is applied in the field of medicine and achieves the effects of simple operation and short analysis time

Active Publication Date: 2017-07-25
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there is no report on chiral separation of methyl 2-(6-hydroxy-2,3-dihydrobenzofuran-3-yl)acetate by capillary electrophoresis at home and abroad

Method used

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  • Chiral resolution method of methyl 2-(6-hydroxy-2, 3-dihydrobenzofuran-3-yl)acetate
  • Chiral resolution method of methyl 2-(6-hydroxy-2, 3-dihydrobenzofuran-3-yl)acetate

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Embodiment

[0024] A chiral resolution method for methyl 2-(6-hydroxy-2,3-dihydrobenzofuran-3-yl)acetate, the steps are as follows:

[0025] a. Sample preparation: Accurately weigh 8 mg of 2-(6-hydroxy-2,3-dihydrobenzofuran-3-yl) methyl acetate racemate powder, place it in a 10 mL volumetric flask, and use filtered Dissolve acetonitrile and adjust the volume to the mark, shake well to obtain a stock solution with a sample concentration of 0.8 mg / mL, and store in a refrigerator at 4°C. Precisely measure 1 mL of the stock solution in a 10 mL volumetric flask, adjust the volume to the mark with buffer solution, and shake well to obtain a 80 μg / mL test solution, which is filtered through a 0.45 μm microporous membrane for use.

[0026] b. Separation steps and conditions: prepare 25mmol / L Na 2 B 4 o 7 Containing 1.8% sulfonic acid-β-cyclodextrin as the running buffer, adjusted to pH 8.9 with boric acid, filtered through a 0.45 μm microporous membrane, and ultrasonically degassed for later u...

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Abstract

The invention discloses a chiral resolution method of methyl 2-(6-hydroxy-2, 3-dihydrobenzofuran-3-yl)acetate. The method utilizes sulfated-beta-cyclodextrin as a selective agent and sodium tetraborate as a buffer liquid. Under the action of sulfated-beta-cyclodextrin, enantiomer baseline separation is realized through capillary electrophoresis. The method has the advantages of simple operation, short analysis time, less use amount of the reagent and no pollution to the environment, and can be used for rapid detection of the optical purity of the compound.

Description

technical field [0001] The invention relates to a method for resolving chiral intermediate impurities in medicines, in particular to a method for chiral resolution of 2-(6-hydroxy-2,3-dihydrobenzofuran-3-yl)acetic acid by capillary electrophoresis The method for methyl ester belongs to the technical field of medicine. Background technique [0002] Methyl 2-(6-hydroxy-2,3-dihydrobenzofuran-3-yl)acetate is an important raw material for the synthesis of GPR40 agonist TAK-875 and its analogues. Its molecular structure contains a chiral center, Controlling the purity of methyl 2-(6-hydroxy-2,3-dihydrobenzofuran-3-yl)acetate plays a very important role in controlling the chiral impurities of the final product. Therefore, it is necessary to establish a method that can rapidly separate methyl 2-(6-hydroxy-2,3-dihydrobenzofuran-3-yl)acetate. [0003] It has been reported in the literature that 2-(6-hydroxy-2, 3-dihydrobenzofuran-3-yl) methyl acetate, but this method has following ...

Claims

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Application Information

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IPC IPC(8): C07D307/79C07B57/00G01N30/02
CPCC07B57/00C07B2200/07C07D307/79G01N30/02
Inventor 杨新颖潘文燕方浩
Owner SHANDONG UNIV