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Method for preparing maltol and homologue thereof by regulating and controlling chlorination-hydrolysis reaction

A technology of hydrolysis reaction and maltol, applied in directions such as organic chemistry, can solve problems such as low yield, and achieve the effects of reducing production cost, not affecting yield, and easily controlling reaction temperature

Active Publication Date: 2019-11-05
河北省天利海香精香料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This reaction has following shortcoming, the productive rate of maltol homologue is relatively low, about 60%, produces the black tar by-product of a large amount of resins about 40%

Method used

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  • Method for preparing maltol and homologue thereof by regulating and controlling chlorination-hydrolysis reaction
  • Method for preparing maltol and homologue thereof by regulating and controlling chlorination-hydrolysis reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A preparation method of methyl maltol, comprising the following steps:

[0025] 1) Put 1 mol of α-furyl methane alcohol in 100 mL of carbon tetrachloride, and then pass through 1 mol of chlorine gas to fully react for 2 hours to generate unstable 2,4-dichloro-α-dihydrofuryl methane alcohol compound;

[0026] 2) Add 55mL of ethanol aqueous solution with 70% ethanol content to the system after the reaction in step 1), and place it at a temperature of 8°C, and react for 50min to generate 6-hydroxy-2-alkyl-1,3-pyridine Ketone compounds;

[0027] 3) Then cool down the reaction system in step 2) to below 0°C, then slowly introduce 1 mol of chlorine gas into the reaction system to generate 2-alkyl-4-chloro-6-hydroxyl-1,3-pyrone compound;

[0028] 4) Slowly heat up the reaction system in step 3) to 60° C., then add 25 mL of ethanol aqueous solution with 50% ethanol content to carry out hydrolysis reaction to obtain methyl maltol.

Embodiment 2

[0030] A preparation method of ethyl maltol, comprising the following steps:

[0031] 1) Put 1 mol of α-furan alcohol in 100 mL of carbon tetrachloride, and then feed 1 mol of chlorine to fully react for 2 hours to generate unstable 2,4-dichloro-α-dihydrofuran alcohol compound;

[0032] 2) Add 55mL of ethanol aqueous solution with 70% ethanol content to the system after the reaction in step 1), and place it at a temperature of 10°C, and react for 60min to generate 6-hydroxy-2-alkyl-1,3-pyridine Ketone compounds;

[0033] 3) Then cool down the reaction system in step 2) to below 0°C, then slowly introduce 1 mol of chlorine gas into the reaction system to generate 2-alkyl-4-chloro-6-hydroxyl-1,3-pyrone compound;

[0034] 4) The system after the reaction in step 3) was slowly heated to 58° C., and then 25 mL of ethanol aqueous solution with an ethanol content of 50% was added for hydrolysis reaction to obtain ethyl maltol.

[0035] After testing, the yields of methyl maltol an...

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Abstract

The invention discloses a method for preparing maltol and a homologue thereof by regulating and controlling a chlorination-hydrolysis reaction. According to the method, by regulating and controlling the chlorination reaction process, the polymerization reaction under the acidic condition of alpha-furanidine is inhibited, the conversion rate of a main reaction is increased, and a target product with high yield is obtained. By adopting the preparation method, the yield of the prepared methyl maltol and the yield of ethyl maltol reach 80% or above, and the generation of byproducts is greatly reduced.

Description

technical field [0001] The invention relates to the technical field of preparation of maltol and its homologues, in particular to a method for preparing maltol and its homologues by regulating and controlling the chlorination-hydrolysis reaction. Background technique [0002] Methyl maltol and ethyl maltol are often added to baked food, ice cream and candy as food flavoring agents, and the amount of maltol added is about 110 μg / kg. According to calculations, the average content of methyl maltol and ethyl maltol The daily intake is 5-29mg, but in some populations, the actual consumption level may be several times the average amount. [0003] At present, the preparation method of methyl maltol and ethyl maltol is to use α-furalkanol and chlorine gas with twice the molecular weight to react in methanol aqueous solution, and then heat and hydrolyze to obtain maltol and its homologues. That is, in a reaction device equipped with a dripping device and chlorine gas, a certain amou...

Claims

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Application Information

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IPC IPC(8): C07D309/40
CPCC07D309/40
Inventor 王军李金合官伟张晓峰于福新宁洪良
Owner 河北省天利海香精香料有限公司
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