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Preparation method of olopatadine hydrochloride

A technology of olopatadine hydrochloride and concentrated hydrochloric acid, which is applied in organic chemistry methods, organic chemistry, etc., can solve problems such as complex reaction routes, achieve high yield, ensure the same quality and yield, and optimize the effect of reaction temperature

Inactive Publication Date: 2019-10-18
重庆西南制药二厂有限责任公司
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Problems solved by technology

[0006] In view of the above-mentioned deficiencies in the prior art, the purpose of the present invention is to provide a preparation method of olopatadine hydrochloride, optimize and upgrade the preparation process, reduce reaction steps, optimize reaction conditions, aim to solve the problem of existing olopatadine hydrochloride The reaction route is too complicated

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  • Preparation method of olopatadine hydrochloride

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Embodiment 1

[0032](1) Add 200g (3-dimethylaminopropyl)triphenylphosphine bromide to the three-necked flask, then add 400g of anhydrous tetrahydrofuran, start stirring, control the temperature at 20~22°C, add 40g of NaH, and raise the temperature after adding To reflux, react for 1h. Then add 100g of isoket acid, reflux and stir for 2 hours, then cool down to 0~15°C, slowly add 30g of anhydrous methanol, then add 400g of tetrahydrofuran aqueous solution with a mass concentration of 50%, and finally add 1600g of water to quench the reaction. The reaction solution was adjusted to PH=6±0.2 with concentrated hydrochloric acid, then distilled to dryness under reduced pressure, and evaporated to dryness to obtain a solid. The solid was dissolved in 1400g of acetone, started stirring, and 40g of concentrated hydrochloric acid was added to precipitate a white solid. After the dropwise addition, the temperature was lowered to 10-15°C and stirred for another 10 hours. Suction filtration to obtain a...

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Abstract

The invention discloses a preparation method of olopatadine hydrochloride. The preparation method comprises the following steps of preparing olopatadine hydrochloride crude products, preparing olopatadine freebase and preparing olopatadine hydrochloride. According to the preparation method of olopatadine hydrochloride, the key steps are upgraded, and the preparation method has the following advantages that 1, reaction steps are reduced, the loss is reduced, and the production efficiency is improved; 2, generation of hydrogen is reduced, and potential safety hazards are reduced; 3, the processing difficulty is reduced while ensuring the quality and yield unchanged; 4, a reaction temperature is optimized, a low-temperature harsh reaction is eliminated, and the dependence on equipment is reduced; 5, an original separate heterogeneous removal step is eliminated; and 6, the yield is high and the quality is good.

Description

technical field [0001] The invention relates to the field of drug synthesis, and mainly relates to a preparation method of olopatadine hydrochloride. Background technique [0002] Olopatadine hydrochloride (Olopatadine hydrochloride) as a new H 1 Receptor antagonist, an excellent allergy drug with oral long-acting, high selectivity, no central inhibition, and no cardiotoxicity. Its chemical name is: (Z)-11-[3-(dimethylamino)propylene]-6,11-dihydrodibenzo[b,e]oxazepine-2-acetic acid hydrochloride , CAS: 140462-76-6. Its structural formula is as follows: [0003] . [0004] At present, the preparation of olopatadine hydrochloride is mainly by chemical synthesis. Some manufacturers use 3,3-dimethylaminopropylmagnesium chloride (CAS: 19070-16-7) and the intermediate isoket acid (CAS: 55453 -87-7) or Grignard reaction with isoket acid with protective group, prepared by deprotection by salt formation, some manufacturers use [3-(dimethylamino)propyl]triphenylphosphine bromid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D313/12
CPCC07B2200/09C07D313/12
Inventor 邹浩胡训刚谭启宣王兴明胡训龙何桥
Owner 重庆西南制药二厂有限责任公司
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