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Synthesis method of N-boc-4-hydroxypiperidine

A technology of n-boc-4-, hydroxypiperidine, applied in the field of medicine, can solve problems such as being unsuitable for industrial production, and achieve the effects of low cost, readily available raw materials and stable properties

Inactive Publication Date: 2015-05-20
ANHUI DEXINJIA BIOPHARM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] N-boc-4-hydroxypiperidine is a pharmaceutical intermediate used to treat anti-tumor and other drugs, and is an important fine chemical intermediate, which has a wide range of uses in the pharmaceutical industry. At present, there are few reports on related synthesis methods, and Not suitable for industrial production

Method used

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  • Synthesis method of N-boc-4-hydroxypiperidine
  • Synthesis method of N-boc-4-hydroxypiperidine

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Embodiment 1

[0015] A kind of N-boc-4-hydroxypiperidine synthetic method is characterized in that comprising the following steps:

[0016] (1) Synthesis of 4-piperidone

[0017] Add 20 grams of 4-piperidone hydrochloride hydrate into a 100 ml three-necked glass bottle, add 30 ml of distilled water, pass through liquid ammonia to make it alkaline, extract it with toluene three times, dry it with anhydrous magnesium sulfate for 12 hours, and suction filter anhydrous magnesium sulfate. Keep the organic phase, concentrate until viscous and set aside to obtain 12 grams;

[0018] (2) Synthesis of 4-hydroxypiperidine

[0019] Add 12 grams of 4-piperidone synthesized above into a 100ml three-necked glass bottle, add 50ml of methanol to dissolve, start stirring, control the temperature at 30°C, add 8 grams of sodium borohydride, control the addition within 30 minutes, and then reflux the reaction 10h, concentrate methanol until a small amount of solid appears, add 5% dilute hydrochloric acid to a...

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Abstract

The invention discloses a synthesis method of N-boc-4-hydroxypiperidine, which comprises the following steps: taking 4-piperidone hydrochloride hydrate, adding distilled water, introducing liquid ammonia to alkalinity, extracting with toluene, drying with anhydrous magnesium sulfate, and carrying out vacuum filtration to obtain 4-piperidone; dissolving in methanol, adding sodium borohydride, refluxing, concentrating, adding dilute hydrochloric acid to regulate the pH value, adding dichloromethane to separate out the water layer, maintaining the organic phase, drying with anhydrous magnesium sulfate over night, carrying out vacuum filtration, maintaining the organic phase, concentrating, adding n-hexane, refrigerating to crystallize, carrying out vacuum filtration, adding methanol, potassium carbonate and di-tert-butyl dicarbonate, refluxing, filtering, concentrating, adding petroleum ether, and refrigerating to crystallize, thereby obtaining the final white crystal product. The method has the advantages of accessible raw materials, high reaction yield, low cost, favorable selectivity and the like, is simple to operate and can easily implement industrialization. The product has the advantages of high purity and stable properties, and completely conforms to the operating requirements as a drug intermediate.

Description

technical field [0001] The invention mainly relates to the field of medicine, in particular to a synthesis method of N-boc-4-hydroxypiperidine. Background technique [0002] N-boc-4-hydroxypiperidine is a pharmaceutical intermediate used to treat anti-tumor and other drugs, and is an important fine chemical intermediate, which has a wide range of uses in the pharmaceutical industry. At present, there are few reports on related synthesis methods, and are not suitable for industrial production. Contents of the invention [0003] The object of the present invention is just to provide a kind of N-boc-4-hydroxypiperidine synthetic method. [0004] The present invention is achieved through the following technical solutions: [0005] A kind of N-boc-4-hydroxypiperidine synthetic method, comprises the following steps: [0006] (1) Synthesis of 4-piperidone [0007] Add 20 grams of 4-piperidone hydrochloride hydrate into a 100ml three-neck glass bottle, add 30ml of distilled wa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D211/46
CPCC07D211/46
Inventor 许坤田玉花
Owner ANHUI DEXINJIA BIOPHARM
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