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Synthesis method of nitrogen-(benzoxycarbonyl piperidine-4-yl)-2-(trifluoromethyl)benzamide

A technology of benzyloxycarbonylpiperidine and trifluoromethyl, which is applied in the field of practical synthesis of nitrogen-2-benzamide, can solve the problems of no industrialized synthetic route report, and achieve the purpose of filling the blank of industrialized synthesis and reaction Reasonable process design to avoid the effect of post-processing

Inactive Publication Date: 2019-03-22
WUXI APPTEC (TIANJIN) CO LTD
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Problems solved by technology

[0002] Nitrogen-(benzyloxycarbonylpiperidin-4-yl)-2-(trifluoromethyl)benzamide, CAS No. 7732-18-5, there is currently no report on an industrialized synthetic route

Method used

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  • Synthesis method of nitrogen-(benzoxycarbonyl piperidine-4-yl)-2-(trifluoromethyl)benzamide

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Embodiment 1

[0009] Synthesis of Nitrogen-(Benzyloxycarbonylpiperidin-4-yl)-2-(trifluoromethyl)benzamide

[0010]

[0011] 3 grams of compound 1 and 4.7 grams of sodium carbonate were added to a mixed solvent of 25 mL of tetrahydrofuran and 25 mL of water, the mixture was cooled to 0 degrees Celsius, and 2 grams of compound 2 was slowly added dropwise to the above suspension under stirring, controlled Throughout the dropping process, the temperature was kept at 0°C. After the dropwise addition was completed, the reaction was carried out at 0° C. for 2 hours.

[0012] After the reaction was completed, the reaction liquid was extracted twice with 50 mL of dichloromethane, the organic phase was collected, washed once with 50 mL of saturated brine, the organic phase was dried with sodium sulfate, filtered and spin-dried to obtain the crude compound 3, and the crude compound 3 was obtained using 30 mL of methyl The tert-butyl ether was beaten, and the solid was collected to obtain 3.4 g of ...

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Abstract

The invention relates to a synthesis method of nitrogen-(benzoxycarbonyl piperidine-4-yl)-2-(trifluoromethyl)benzamide. The technical problem that the compound did not have the industrialized synthesis route report before is mainly solved. According to the technical scheme of the invention, the synthesis method of the nitrogen-(benzoxycarbonyl piperidine-4-yl)-2-(trifluoromethyl)benzamide comprises the following steps: adding nitrogen-(piperidine-4-yl)-2-(trifluoromethyl)benzamide and sodium carbonate into tetrahydrofuran and water, adding benzyl chloroformate slowly and dropwise, performing reaction, and performing aftertreatment to obtain the nitrogen-(benzoxycarbonyl piperidine-4-yl)-2-(trifluoromethyl)benzamide. The cheap and easily available raw materials are adopted, so that the complicated aftertreatment process is avoided; and the target molecule is obtained only through one-step reaction, so that amplification is facilitated.

Description

technical field [0001] The invention relates to a practical synthesis method of nitrogen-(benzyloxycarbonylpiperidin-4-yl)-2-(trifluoromethyl)benzamide. Background technique [0002] Nitrogen-(benzyloxycarbonylpiperidin-4-yl)-2-(trifluoromethyl)benzamide, CAS No. 7732-18-5, currently has no industrialized synthetic route report. Contents of the invention [0003] The purpose of this invention is to develop a kind of simple, general nitrogen-(benzyloxycarbonyl piperidin-4-yl)-2-(trifluoromethyl) benzamide synthetic method, mainly solve the technology that does not have industrialized synthetic route at present question. [0004] Technical scheme of the present invention: a kind of synthetic method of nitrogen-(benzyloxycarbonylpiperidin-4-yl)-2-(trifluoromethyl)benzamide, nitrogen-(piperidin-4-yl)-2 -(trifluoromethyl)benzamide and sodium carbonate were added to tetrahydrofuran and water, benzyl chloroformate was slowly added dropwise, and the reaction was post-treated to ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D211/58
CPCC07D211/58
Inventor 林琦森甄蕊张静波刘小丽柴艳萍朱喜雯吴璇刘颖哈维杰李磊
Owner WUXI APPTEC (TIANJIN) CO LTD
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