Synthesis method and device of 2,3,5,6-tetramethylpyrazine

A technology of tetramethylpyrazine and synthetic methods, applied in the direction of organic chemistry, etc., can solve the problems of high operating conditions, high production costs, and difficulty in separation, and achieve the effects of low raw material cost, high yield, and low cost

Pending Publication Date: 2018-11-23
WUTONG AROMA CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, the existing synthesis method requires relatively high operating conditions, and there are many by-products, which are difficult to separate; at the same time, the production cost of the existing method is relatively high, and the yield is relatively low

Method used

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  • Synthesis method and device of 2,3,5,6-tetramethylpyrazine
  • Synthesis method and device of 2,3,5,6-tetramethylpyrazine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Prepare the pipeline reactor, condenser, metering pump and reaction kettle equipped with elevated tank and bubbling device;

[0056] Heat the reactor water bath to 80°C, prepare a mixed aqueous solution of acetoin, ammonium acetate and sodium acetate, and add it to the batching kettle; the molar ratio of acetoin and ammonium acetate is 1:1.15;

[0057] Use the metering pump to transfer the reaction liquid to the head tank, and then enter the radial adiabatic fixed bed reactor through the metering pump in the head tank;

[0058] The temperature of the water bath is raised to 80°C, and at the same time, the bubbler is turned on, and the air is blown into the pipeline for reaction. When the content of 2,3,5,6-tetramethylpyrazine in the material reaches the preset value, the material is transferred to the neutralization Carry out post-processing in the freezer;

[0059] The post-treated material is separated by a centrifugal separation device to recover the solid product, ...

Embodiment 2

[0063] Prepare the pipeline reactor equipped with elevated tank and bubbling device, condenser, metering pump and reactor;

[0064] Heat the reactor water bath to 80°C, prepare a mixed aqueous solution of acetoin, ammonium acetate and sodium acetate, and add it to the batching kettle; the molar ratio of acetoin and ammonium acetate is 1:1.2;

[0065] Use the metering pump to transfer the reaction liquid to the head tank, and then enter the radial adiabatic fixed bed reactor through the metering pump in the head tank;

[0066] The temperature of the water bath is raised to 80°C, and at the same time, the bubbler is turned on, and the air is blown into the pipeline for reaction. When the content of 2,3,5,6-tetramethylpyrazine in the material reaches the preset value, the material is transferred to the neutralization Carry out post-processing in the freezer;

[0067] The post-treated material is separated by a centrifugal separation device to recover the solid product, and the c...

Embodiment 3

[0071] Prepare the pipeline reactor, condenser, metering pump and reaction kettle equipped with elevated tank and bubbling device;

[0072] Heat the reactor water bath to 80°C, prepare a mixed aqueous solution of acetoin, ammonium acetate and sodium acetate, and add it to the batching kettle; the molar ratio of acetoin and ammonium acetate is 1:1.18;

[0073] Use the metering pump to transfer the reaction liquid to the head tank, and then enter the radial adiabatic fixed bed reactor through the metering pump in the head tank;

[0074] The temperature of the water bath is raised to 80°C, and at the same time, the bubbler is turned on, and the air is blown into the pipeline for reaction. When the content of 2,3,5,6-tetramethylpyrazine in the material reaches the preset value, the material is transferred to the neutralization Carry out post-processing in the freezer;

[0075] The post-treated material is separated by a centrifugal separation device to recover the solid product, ...

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Abstract

The invention provides a synthesis method and device of 2,3,5,6-tetramethylpyrazine. The synthesis method provided by the invention comprises: under the air oxidation condition, performing a reactionof acetoin in buffer solution and ammonium salt to obtain the 2,3,5,6-tetramethylpyrazine. In the method provided by the invention, under the condition of a buffer system, acetoin and ammonium salt are used as the raw materials to carry out production. The synthesis method and device are not only low in raw material cost, but also simple and convenient in reaction step, can also implement recycling of the raw materials and a solvent so as to obtain the 2,3,5,6-tetramethylpyrazine in a high-yield low-pollution low-cost mode.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a synthesis method and device for 2,3,5,6-tetramethylpyrazine. Background technique: [0002] 2,3,5,6-Tetramethylpyrazine, the English name is 2,3,5,6-tetramethylpyrazine TMP, also known as Ligustrazine. As the active ingredient of the traditional Chinese medicine Chuanxiong, 2,3,5,6-tetramethylpyrazine is an important pharmaceutical intermediate, which was first extracted from the dried rhizome of Ligusticum chuanxiong in the Umbelliferae family. Since the quantity extracted from natural products cannot meet the requirements of the market, the alkaloid monomer is mostly obtained by artificial synthesis. [0003] 2,3,5,6-Tetramethylpyrazine has a wide range of medicinal uses. It is reported that it has a good effect on anti-platelet aggregation and deaggregation. By dilating small arteries, 2,3,5,6-tetra Methylpyrazine can significantly improve microcirculation, cerebral blood ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D241/12
CPCC07D241/12
Inventor 陈祥臧传近卫洁宋成斌李磊磊张广军闫培良郭鸽张雷亮王新军
Owner WUTONG AROMA CHEM CO LTD
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