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Method for purifying 2-[(4-chlorophenyl)(piperidin-4-yloxy)methyl]pyridine

A compound and organic solvent technology, applied in the field of high-purity products, can solve the problems of cumbersome industrial production, inability to continue, and time-consuming crystallization process, and achieve the effect of shortening purification time and high purity

Inactive Publication Date: 2014-07-16
CHONGQING HUAPONT PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Although this method precipitates the salt of formula I through salt formation, and indirectly removes impurities, but due to the crystallization process in the middle, it is relatively cumbersome during industrial production.
Moreover, the crystallization process takes a long time, and often takes several hours to tens of hours, resulting in the inability to continue industrial production;

Method used

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  • Method for purifying 2-[(4-chlorophenyl)(piperidin-4-yloxy)methyl]pyridine
  • Method for purifying 2-[(4-chlorophenyl)(piperidin-4-yloxy)methyl]pyridine
  • Method for purifying 2-[(4-chlorophenyl)(piperidin-4-yloxy)methyl]pyridine

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Effect test

Embodiment 1

[0048] Embodiment 1 Purification of Formula I (1)

[0049] Take 20 g of the crude product of formula I, dissolve it with dichloromethane, then add 5% hydrochloric acid to the solution to make the pH of the system 6.2, mix well and make it layered. The organic layer was discarded, and the pH value of the aqueous layer was adjusted to 10.0 with sodium hydroxide, then extracted with an appropriate amount of dichloromethane, the extract was dried, filtered, and concentrated to obtain 14.6 g of a red viscous liquid with a purity of 98.8%.

Embodiment 2

[0050] The purification of embodiment 2 formula I (two)

[0051] Add 20ml of diethyl ether to 400ml of water, then use glacial acetic acid to adjust the pH value of the system to 5.0, add 15g of the crude product of formula I to the above system to dissolve, mix well and make it layered. Separate the water layer, adjust the pH value to 8.5 with ammonia water, extract with an appropriate amount of chloroform, dry the extract, filter, and concentrate to obtain 15.8 g of red viscous liquid with a purity of 99.1%.

Embodiment 3

[0052] The purification of embodiment 3 formula I (three)

[0053] Take 15g of the crude product of formula I, dissolve it with toluene, add 160ml of water to the solution, then use 10% p-toluenesulfonic acid to adjust the pH value of the system to 8.0, mix well and make it layered, discard the organic layer, and use hydrogen After the pH value was adjusted to 14.0 with lithium oxide, it was extracted with an appropriate amount of toluene, and the extract was dried, filtered, and concentrated to obtain 12.0 g of a red viscous liquid with a purity of 98.2%.

[0054] The purification of embodiment 4 formula I (four)

[0055] Take 30g of the crude product of formula I, dissolve it with ethyl acetate, add 15ml of water to the solution, then use 10% sulfuric acid to adjust the pH value of the system to 7.4, mix well and make it layered. The aqueous layer was separated and adjusted to pH 12.0 with potassium oxide, then extracted with an appropriate amount of ethyl acetate, the extr...

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Abstract

The invention relates to a method for purifying 2-[(4-chlorophenyl)(piperidin-4-yloxy)methyl]pyridine. The method comprises: placing a crude product to be purified in a water and organic solvent double phase system having the specific pH value, separating the double phase system to obtain a water phase, adjusting the pH value of the water phase to achieve an alkaline state, and extracting with an organic solvent to obtain the high purity 2-[(4-chlorophenyl)(piperidin-4-yloxy)methyl]pyridine. With the method, the crystallization step in the prior art is eliminated, continuous operation can be achieved, the purity of the obtained product achieves more than 98%, and the obtained product can be used directly in the next step for drug preparation. The method has advantages of simpleness, efficiency, easy industrial application and the like.

Description

technical field [0001] The present invention relates to a kind of preparation method of drug bepotastine intermediate 2-[(4-chlorophenyl)(piperidine-4-oxyl)methyl]pyridine, especially can obtain high Methods of Purity Products. Background technique [0002] 2-[(4-chlorophenyl)(piperidine-4-oxyl)methyl]pyridine (formula I) is an important intermediate for the preparation of antihistamine bepotastine, such as an iso After the conformation is alkylated, bepotastine is obtained. [0003] [0004] JP10120677 introduces the preparation method of formula I to obtain the colorless viscous oily substance formula I, but this document does not disclose the purity and purification method of the product. [0005] The key to the purification of chemical substances is how to remove impurities. The substance formula I of the present invention is itself an oily substance, which is closely combined with impurities. [0006] JP6336480 provides a method for three-step purification of for...

Claims

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Application Information

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IPC IPC(8): C07D401/12
CPCC07D401/12
Inventor 张波邹长忠赵舟
Owner CHONGQING HUAPONT PHARMA
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