Method for synthesizing 1-BOC-3-piperidone

A 1-BOC-3-, piperidinone technology, applied in the field of medicine, can solve problems such as being unsuitable for industrial production, a large amount of waste water, waste residue, complicated operation process, etc., and achieve the effects of mild conditions, short synthesis steps and good purity

Inactive Publication Date: 2013-09-18
YANGZHOU TIANHE PHARM CO LTD
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Problems solved by technology

[0005] The synthesis yield of the above method is low (about 40%), the operation process is complicated, and a large amount of waste water and waste residue are generated during the reaction process, which is very unfriendly to the environment and is not suitable for industrial production.

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  • Method for synthesizing 1-BOC-3-piperidone

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[0022] The following examples are used to further illustrate the present invention, but it should not be interpreted as that the scope of the above-mentioned themes of the present invention is limited to the following examples, and all technologies realized based on the above-mentioned content of the present invention all belong to the scope of the present invention.

[0023] 1. Synthesis of Step 1 compound 2 (3-hydroxypiperidine):

[0024] 1. Preparation of sodium borohydride solution: 113.5g of sodium borohydride, 150ml of water and 40ml of 20% NaOH aqueous solution were mixed.

[0025] 2. Synthesis: Put 95.1g of compound 1 (3-hydroxypyridine) into a 1L reaction flask, add 300ml of NaOH aqueous solution with a mass percentage of 20%, raise the temperature to 60°C, add sodium borohydride solution dropwise, keep warm for 1h, drop After the addition, the temperature was raised to 80°C and kept for 5 hours. After the heat preservation was completed, stirred and cooled to room te...

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Abstract

The invention relates to a method for synthesizing 1-BOC-3-piperidone and relates to a chemical synthesis method of 1-BOC-3-piperidone, belonging to the technical field of medicines. The method comprises the following steps of: with 3-hydroxypyridine as a raw material, reducing the 3-hydroxypyridine, protecting piperidine cyclo-nitrogen BOC, and oxidizing oppenauer to prepare a crude product of the 1-BOC-3-piperidone; and then, carrying out reduced pressure distillation to obtain a fine product of the 1-BOC-3-piperidone. The invention provides the high-efficiency and low-pollution method for synthesizing the 1-BOC-3-piperidone; and the method is simple and convenient to operate, short in synthesis step, mild in condition, environment-friendly in reaction process, high in product yield, good in purity and suitable for industrial production.

Description

technical field [0001] The invention relates to a chemical synthesis method of 1-BOC-3-piperidone, which belongs to the technical field of medicine. Background technique [0002] 1-BOC-3-piperidone, also known as N-tert-butoxycarbonyl-3-piperidone, the molecular formula is C 10 h 17 NO 3 , the structural formula is as follows: [0003] 5. BOC-3-piperidone is a key intermediate in organic synthesis, and it is widely used in organic synthesis, especially in drug synthesis and natural product synthesis. At present, there are few reports about the synthesis of 1-boc-piperidone, and the common synthesis method is shown in the following formula: [0004] [0005] The synthesis yield of the above method is low (about 40%), the operation process is complicated, and a large amount of waste water and waste residue are generated during the reaction process, which is very unfriendly to the environment and is not suitable for industrial production. Contents of the invention ...

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D211/74
Inventor 赵云德庄卫东陶建华
Owner YANGZHOU TIANHE PHARM CO LTD
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