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Preparation method of alcaftadine and purification method of intermediate of alcaftadine

A technology of alcaftadine and intermediates, which is applied in the field of preparation of high-content raw materials, can solve problems such as quality improvement, and achieve the effect of stable purity and good stability

Pending Publication Date: 2022-06-07
WUHAN WUYAO SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no effective method for purifying the intermediate AT3 in the prior art. In addition, the quality of alcatadine in the prior art also needs to be improved

Method used

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  • Preparation method of alcaftadine and purification method of intermediate of alcaftadine
  • Preparation method of alcaftadine and purification method of intermediate of alcaftadine
  • Preparation method of alcaftadine and purification method of intermediate of alcaftadine

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preparation example Construction

[0049] The preparation method of the acarbazide product

[0050] In the first aspect of the present invention, the present invention proposes a preparation method of acapatadine. According to an embodiment of the present invention, it is obtained by oxidizing AT3 through Dess-Martin reagent, and the oxidation reaction includes: combining AT3 and Part of the Dess-Martin reagent is oxidized, and after the oxidation reaction is carried out for a period of time, the remaining Dess-Martin reagent is added; preferably, the weight of the part of the Dess-Martin reagent is the total amount of the Dess-Martin reagent added 0.3 to 0.7 times,

[0051] Wherein, described AT3 is the compound shown in formula (I):

[0052]

[0053] The oxidizing agent Dess-Martin reagent was added in portions.

[0054] According to the embodiment of the present invention, the quality of the additive is controlled to be 0.005 to 0.02 times the mass of AT3;

[0055] According to the embodiment of the pr...

Embodiment 1

[0083] AT3 is prepared from AT2, and its chemical formula is as follows:

[0084]

[0085] The concrete operation steps are as follows: add 2.2kg AT2, acetic acid (0.55kg), 37% formaldehyde solution (6L), and 1.25kg of anhydrous sodium acetate into the reactor, heat to 80~100° C., stir for 18~30 hours, The reaction mixture was cooled to 25-30°C. Dichloromethane (22 L) was added to the reaction mixture and stirred for 30 minutes. The pH of the aqueous layer was adjusted to 8-11 with 20% sodium hydroxide. Stirring was continued for 0.5 hour, the organic layer was separated, the organic layer was washed twice with 20% sodium hydroxide solution, stirred evenly with anhydrous sodium sulfate, and left to dry. Suction filtration, the gained filtrate is concentrated under reduced pressure at 35~45 ℃ until there is solid precipitation, suction filtration, the obtained filter cake is the crude product containing AT3, in the crude product containing AT3, AT3 purity is 77.98%, AT2 re...

Embodiment 2

[0087] The general idea of ​​the following experimental group and comparative group is: carry out slurry washing treatment on the crude product containing AT3 prepared in Example 1, so as to obtain purified AT3.

[0088] Experimental group 1

[0089] The crude product (AT3 content 77.98%, AT2 residual 19.16%, impurity C content is 2.86%) 20g containing AT3 of embodiment 1 gained, the methylene chloride of 80g, the pH of 320g are that the potassium carbonate aqueous solution of 10 is added in the 1L there-necked flask , heated to 30°C, stirred for 1 hour, filtered while hot, and dried the filter cake to obtain purified AT3 with a yield of 96.1%. In the purified AT3, the content of AT3 was 98.98%, the residual AT2 was 0.74%, and the content of impurity C was 0.28%.

[0090] Experimental group 2

[0091] The crude product containing AT3 obtained in Example 1 (AT3 content 77..98%, AT2 residual 19.16%, impurity C content 2.86%) 20g, 60g of dichloromethane, 420g of pH 8 sodium bic...

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Abstract

The invention relates to a method for preparing alcaftadine and a method for purifying an intermediate, which comprises the following steps: washing and separating a crude product containing 6, 11-dihydro-11-(1-methyl-4-piperidino)-5H-imidazo [2, 1-b] [3] benzazepine-3-methanol (abbreviated as AT3) to obtain the purified AT3. Furthermore, the invention also provides a method for preparing the alcaftadine. Through the AT3 purification method provided by the invention, the AT3 purity can be controlled to be 95% or above. The purity of the alcaftadine obtained by the method disclosed by the invention is 99.5% or above.

Description

technical field [0001] The invention relates to a preparation method of a high-content bulk drug, in particular to a preparation method of alcastatine and a method for purifying an intermediate thereof. Background technique [0002] Alcaftadine, trade name: Lastacaft, is a new type of histamine H1 receptor antagonist and mast cell stabilizer developed by Weikang Pharmaceuticals, which can inhibit the release of histamine from mast cells and reduce eosinophilia The chemotaxis and activation of granulocytes was approved by the US FDA in July 2010 under the trade name of Lastacaft. Acatadine is another drug for the treatment of allergic conjunctivitis-related eye pruritus after betaxel besylate developed by ISTA Pharmaceuticals. The drug is an eye drop for allergic conjunctiva in people over 2 years old Treatment of inflammation-related ocular itching. It has good clinical application prospects. Its structural formula is as follows: [0003] [0004] U.S. Patent Applicat...

Claims

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Application Information

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IPC IPC(8): C07D487/04
CPCC07D487/04Y02P20/55
Inventor 宁东波田俊锋陈彦朱毅殷晶莉蔡超
Owner WUHAN WUYAO SCI & TECH
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