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Deuterated piperazine and preparation method thereof

A technology of deuterated piperazine and piperazine, applied in the field of isotope chemicals and preparation, can solve problems such as undiscovered preparation method of deuterated piperazine, and achieve the effect of simple operation

Inactive Publication Date: 2018-01-19
天津莱茵泰克生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Piperazine is already a commercialized chemical product, and its conventional synthesis process has been reported in many literatures, but deuterated piperazine and related preparation methods have not been found
The present invention provides a method for hydrogen-deuterium replacement under high temperature and high pressure conditions, thereby obtaining deuterated piperazine with a high deuteration rate. The high temperature and high pressure conditions here are generally called hydrothermal synthesis in the field of chemical synthesis. The synthesis method is generally used in the field of inorganic chemistry to prepare ultrafine powders, oxide films, and crystal materials, etc. It has not been reported in the replacement of hydrogen and deuterium.

Method used

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  • Deuterated piperazine and preparation method thereof
  • Deuterated piperazine and preparation method thereof
  • Deuterated piperazine and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0032] The preparation method of deuterated piperazine, comprises the steps,

[0033] (1) Put piperazine in the liner of polytetrafluoroethylene reactor, then add deuterated methanol CD 3 OD;

[0034] (2) Put the above-mentioned liner into the supporting stainless steel kettle body, and tighten the lid of the kettle with bolts;

[0035] (3) Continuous heating at high temperature, the heating temperature is controlled at 100°C, and the heating time is controlled at 96h;

[0036] (4) After the heating is completed, the polytetrafluoroethylene reactor is naturally cooled to room temperature, then the reaction system in the liner is transferred to a single-necked flask, and concentrated under reduced pressure until there is no solvent to obtain deuterated piperazine.

[0037] The deuterated piperazine prepared according to the technical solution of the present embodiment adopts gas chromatography to measure the deuterated piperazine purity to be 91.76%.

Embodiment 2

[0039] The preparation method of deuterated piperazine, comprises the steps,

[0040] (1) Put piperazine in the liner of polytetrafluoroethylene reactor, then add deuterated methanol CD 3 OD;

[0041] (2) Put the above-mentioned liner into the supporting stainless steel kettle body, and tighten the lid of the kettle with bolts;

[0042] (3) Continuous heating at high temperature, the heating temperature is controlled at 150°C, and the heating time is controlled at 72h;

[0043] (4) After the heating is completed, the polytetrafluoroethylene reactor is naturally cooled to room temperature, then the reaction system in the liner is transferred to a single-necked flask, and concentrated under reduced pressure until there is no solvent to obtain deuterated piperazine.

[0044] The deuterated piperazine prepared according to the technical solution of the present embodiment adopts gas chromatography to determine that the deuterated piperazine purity is 92.44%.

Embodiment 3

[0046] The preparation method of deuterated piperazine, comprises the steps,

[0047] (1) Put piperazine in the liner of polytetrafluoroethylene reactor, then add deuterated methanol CD 3 OD;

[0048] (2) Put the above-mentioned liner into the supporting stainless steel kettle body, and tighten the lid of the kettle with bolts;

[0049] (3) Continuous heating at high temperature, the heating temperature is controlled at 200°C, and the heating time is controlled at 48h;

[0050] (4) After the heating is completed, the polytetrafluoroethylene reactor is naturally cooled to room temperature, then the reaction system in the liner is transferred to a single-necked flask, and concentrated under reduced pressure until there is no solvent to obtain deuterated piperazine.

[0051] The purity of the deuterated piperazine obtained according to the technical solution of the present embodiment is 92.46% by gas chromatography.

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Abstract

The invention provides deuterated piperazine and a preparation method of the deuterated piperazine, and fills up the technical blank of deuteration of piperazine. The preparation method comprises thefollowing steps: putting piperazine into a liner of a polytetrafluoroethylene reaction kettle, and adding a deuterated reagent; putting the liner into a matched stainless steel kettle body, and tightening a kettle cover by using a bolt; continuously heating at high temperature, controlling the heating temperature to 100-250 DEG C, and controlling the heating time to 24-96 hours; and naturally cooling the polytetrafluoroethylene reaction kettle to the room temperature after finishing heating, transferring a reaction system in the liner to a single-neck flask, conducting vacuum concentration until no solvent exists, and obtaining deuterated piperazine. The molecular structure of the deuterated piperazine is shown in the description.

Description

technical field [0001] The invention belongs to the field of isotope chemicals and preparation technology, in particular, relates to deuterated piperazine and a preparation method. Background technique [0002] Deuterium (deuterium, D) is a stable non-radioactive isotope of hydrogen, also known as heavy hydrogen. There is a proton and a neutron in the deuterium nucleus, and its relative atomic weight is twice that of ordinary hydrogen. There is 0.02% deuterium in hydrogen element, which is about 1 / 7000 of ordinary hydrogen in nature. [0003] Since the carbon-deuterium bond is more stable than the carbon-hydrogen bond, in the field of biomedicine, the hydrogen atoms in some positions in the drug molecule are replaced by its stable isotope deuterium, that is, the deuterium labeling of the drug can directly affect the drug. The process of absorption, distribution, metabolism and excretion, on the one hand, can improve the curative effect, and on the other hand, can quickly ob...

Claims

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Application Information

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IPC IPC(8): C07D295/023C07D295/027
Inventor 张宇
Owner 天津莱茵泰克生物科技有限公司
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