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Preparation method of 3-(difluoromethoxy) piperidine hydrochloride

A technology of difluoromethoxy and hydrochloride, applied in the field of synthesis of 3-piperidine hydrochloride, can solve problems such as no suitable industrial synthesis method, and achieve the effects of short synthesis route, easy reaction and convenient operation

Inactive Publication Date: 2019-04-16
WUXI APPTEC (TIANJIN) CO LTD
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

Mainly solve the technical problem that there is no suitable industrial synthesis method at present

Method used

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  • Preparation method of 3-(difluoromethoxy) piperidine hydrochloride
  • Preparation method of 3-(difluoromethoxy) piperidine hydrochloride

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Experimental program
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Embodiment 1

[0011] Add compound 1 (50 g, 248.4 mmol) into acetonitrile (70 mL), then add cuprous iodide (9.5 g, 49.7 mmol), heat the reaction to 50 ° C, and then add dropwise to the reaction solution previously dissolved in acetonitrile (30 mL) of 2-(fluorosulfonyl)difluoroacetic acid and the reaction was stirred continuously at 50°C for 1 hour. TLC (petroleum ether / ethyl acetate volume ratio=3 / 1) showed that the reaction was complete. The solvent in the reaction system was removed by concentration, then water (50 mL) was added, extracted with ethyl acetate, dried over anhydrous sodium sulfate, concentrated under reduced pressure to obtain a crude product, which was separated and purified by column chromatography to obtain 4.5 g of compound 2, yield It was 72.09%.

[0012] Compound 2 (20 g, 79.6 mmol) was added into ethyl acetate (50 mL), ethyl acetate hydrochloride (4M, 300 mL) was added, and the reaction was continuously stirred at 15°C for 2 hours. LC (petroleum ether / ethyl acetate v...

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Abstract

The invention relates to a preparation method of 3-(difluoromethoxy) piperidine hydrochloride. The main technical problem is solved that in the prior art, no suitable industrialized synthesis method exists. The preparation method comprises the two steps that in the first step, a compound 1 is added into acetonitrile, copper iodide is added into a solution, a mixture is heated, then 2-(fluorosulfonyl) difluoroacetic acid, and after a reaction is ended, a compound 2 is obtained through purification of after-treatment; in the second step, the compound 2 is stirred in an ethyl acetate hydrochloride solution to obtain a compound 3, wherein the reaction formula is shown in the specification. The obtained compound is an intermediate or a product which is synthesized by many medicines.

Description

technical field [0001] The invention relates to a synthesis method of 3-(difluoromethoxy)piperidine hydrochloride (CAS: 1638772-02-7). Background technique [0002] 3-(Difluoromethoxy)piperidine hydrochloride and related derivatives are widely used in medicinal chemistry and organic synthesis. At present, there are few reports on the synthesis of 3-(difluoromethoxy)piperidine hydrochloride, and the reactions in similar literatures are dangerous and have long routes and low yields. Therefore, it is necessary to develop a synthetic method with easy-to-obtain raw materials, convenient operation, easy-to-control reaction and suitable overall yield. Contents of the invention [0003] The purpose of the invention is to develop a kind of synthetic method that has raw material easy to get, easy to operate, easy to control reaction, higher yield of 3-(difluoromethoxy)piperidine hydrochloride. It mainly solves the technical problem that there is no suitable industrial synthesis me...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D211/42
CPCC07D211/42
Inventor 吴东平周强任文武李红何米娜蒋欣欣李庆攀何华敬安自强刘月领吴艳何燕平焦家盛于凌波马汝建
Owner WUXI APPTEC (TIANJIN) CO LTD
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