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Preparation method of 1-t-butyloxycarboryl-4-piperidinol

A technology of tert-butoxycarbonyl and piperidinol, which is applied in the field of biopharmaceuticals, can solve the problems of dependence on imports, and the synthesis method of 1-tert-butoxycarbonyl-4-piperidinol has no literature reports, and achieves guaranteed purity and simple steps , the effect of increasing the yield

Inactive Publication Date: 2017-05-10
ABA CHEM SHANGHAI
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Problems solved by technology

my country's annual demand is relatively large, but most of them rely on imports. After searching, there is no literature report on the synthesis method of 1-tert-butoxycarbonyl-4-piperidinol in China.

Method used

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  • Preparation method of 1-t-butyloxycarboryl-4-piperidinol
  • Preparation method of 1-t-butyloxycarboryl-4-piperidinol

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preparation example Construction

[0012] The preparation method of 1-tert-butoxycarbonyl-4-piperidinol of the present invention, the specific steps of the preparation method are as follows: in an organic solvent and carbon dioxide, 1-tert-butoxycarbonyl-4-piperidone is heated at 5 to 10°C by NaBH 4 Reduction gives 1-tert-butoxycarbonyl-4-piperidinol, the NaBH 4 The molar ratio to 1-tert-butoxycarbonyl-4-piperidone is 0.71-0.75:1.

[0013] As an example, a more specific embodiment is that the organic solvent is an alcoholic solvent, and the alcoholic solvent is methanol or ethanol; the reduction reaction time is 2-4 hours.

Embodiment 1

[0015] Dissolve 1 mol of 1-tert-butoxycarbonyl-4-piperidone in 120 ml of methanol, and press it to 40 kg with carbon dioxide, then add NaBH after cooling to 5°C in an ice bath 4 0.71mol, keep the temperature at 5-10°C for 2 hours, slowly rise to room temperature after the reaction, remove methanol by distillation under reduced pressure, then extract the residue with ethyl acetate, and obtain the product after removing ethyl acetate from the extract .

Embodiment 2

[0017] Dissolve 1 mol of 1-tert-butoxycarbonyl-4-piperidone in 120 ml of methanol, and press it to 40 kg with carbon dioxide, then add NaBH after cooling to 10°C in an ice bath 4 0.75mol, keep the temperature at 5-10°C for 4 hours, slowly rise to room temperature after the reaction, remove methanol by distillation under reduced pressure, then extract the residue with ethyl acetate, and then obtain the product after removing ethyl acetate from the extract .

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Abstract

The invention relates to a preparation method of 1-t-butyloxycarboryl-4-piperidinol. The preparation method comprises a following step: in an organic solvent and carbon dioxide, 1-t-butyloxycarboryl-4-piperidone is subjected to reduction with NaBH4 at 5 to 10 DEG C so as to obtain 1-t-butyloxycarboryl-4-piperidinol, wherein the molar ratio of NaBH4 to 1-t-butyloxycarboryl-4-piperidone is controlled to be 0.71-0.75:1. The preparation method possesses following advantages: high purity 1-t-butyloxycarboryl-4-piperidone containing C=O bonds is taken as the raw material, selective reduction of the C=O bonds on piperidine rings with NaBH4 is realized, product purity is ensured, the organic solvent and carbon dioxide are mixed for reaction, product yield is increased greatly to be 80% or higher, and the preparation method is simple, and is suitable for industrialized large-scale production.

Description

technical field [0001] The invention belongs to the technical field of biopharmaceuticals, and relates to a preparation method of a drug intermediate, in particular to a preparation method of 1-tert-butoxycarbonyl-4-piperidinol. Background technique [0002] 1-tert-butoxycarbonyl-4-piperidinol is a very important intermediate of medicine, pesticide and other chemical additives. my country's annual demand is relatively large, but most of them rely on imports. After searching, there is no literature report on the synthesis method of 1-tert-butoxycarbonyl-4-piperidinol in China. [0003] However, after retrieval, the preparation of 1-tert-butoxycarbonyl-4-piperidinone, a derivative of 1-tert-butoxycarbonyl-4-piperidinol, has been reported, and the patent CN 102070513 B discloses 1-tert-butoxycarbonyl -The synthetic method of 4-piperidone, dissolving benzylamine and methyl acrylate with methanol, carrying out Michael addition reaction at room temperature, removing methanol, and...

Claims

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Application Information

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IPC IPC(8): C07D211/46
CPCC07D211/46
Inventor 张敏华毛建勇肖方亮周宇
Owner ABA CHEM SHANGHAI
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