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Preparation method of 2, 3, 5-trimethylpyrazine

A technology of trimethylpyrazine and hydroxyl group, applied in the field of food additives, can solve the problems of restricting the mass use of modified products and high price, and achieve the effects of high yield, low cost and high product purity

Inactive Publication Date: 2011-01-26
杨亮
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  • Summary
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AI Technical Summary

Problems solved by technology

Among the above three methods, the prices of "2.3-butanedione", "2.3 butylene oxide" and "2.3 butanediol" are relatively high, which limits the large-scale use of modified products

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0006] Example 1: Lower the temperature of the low-temperature tank to -5~0°C, add 150ml of water, 220g of 1.2 propylenediamine, control the inner temperature of the bottle at 0~15°C, and add 250g of "3-hydroxy-2-butanone" dropwise , stirred and reacted for 0.5 hour; remove the low-temperature tank, change the heating mantle and heat the bottle to reflux, then drop to room temperature to obtain the reaction mother liquor; zinc oxide catalyst is filled in the stainless steel fixed-bed reactor (Dg25*1000mm), first activated with hydrogen, Then raise the column temperature of the reactor to 350°C, feed the reaction mother liquid, control the column temperature to 340-370°C, flow rate 250ml / h, and continue to pass 100ml of water after passing through; collect the above reaction liquid, and then extract it with 100ml*3 ether, Combine diethyl ether and heat to remove ether to a bottom temperature of 80°C to obtain 380 grams of crude product "2.3.5-trimethylpyrazine" with a content of...

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PUM

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Abstract

The invention discloses a preparation method of 2, 3, 5-trimethylpyrazine. In the invention, low-cost chemical raw materials (3-hydroxy-2-butanone and 1, 2-propane diamine) are used for synthesizing the product of 2, 3, 5-trimethylpyrazine by controlling reaction conditions with high selectivity. The preparation method of 2, 3, 5-trimethylpyrazine is characterized by comprising the following steps of: reducing the temperature of a low-temperature bath to -5-0 DEG C, adding 150ml of water and 220g of 1,2 propane diamine, controlling the temperature in a bottle to be 0-15 DEG C, dropwise adding 250g of 3-hydroxy-2-butanone, and stirring to react for 0.5h. The product of 2, 3, 5-trimethylpyrazine can be synthesized with high selectivity by controlling the reaction conditions.

Description

technical field [0001] "2.3.5-Trimethylpyrazine" is mainly used as a food additive. It has a special aroma of roasted nuts and belongs to the technical field of food additives. Background technique [0002] At present, the preparation methods of "2.3.5-trimethylpyrazine" mainly include the following three methods: a. Condensation and dehydrogenation of "2.3-butanedione" and "1.2-propylenediamine"; b. "2.3- Addition of "butylene oxide" and "1.2-propylenediamine", followed by dehydration and dehydrogenation; c. Prepared by dehydration and dehydrogenation of "2.3-butanediol" and "1.2-propylenediamine". Among the above three methods, the prices of "2.3-butanedione", "2.3 butylene oxide" and "2.3 butanediol" are relatively high, which limits the large-scale use of modified products. Contents of the invention [0003] The invention provides a preparation method of "2.3.5-trimethylpyrazine", which adopts low-cost chemical raw materials ("3-hydroxy-2-butanone" and "1.2-propylened...

Claims

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Application Information

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IPC IPC(8): C07D241/12
Inventor 杨亮
Owner 杨亮
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