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Grignard reagent synthesis reaction solvent in maltol production

A Grignard reagent and synthetic reaction technology, applied in the field of Grignard reagent synthetic reaction solvent, can solve the problems of high production cost, difficult process control, high product toxicity, etc., and achieve low production cost, low toxicity and normal production operation Effect

Inactive Publication Date: 2008-02-20
ANHUI JINGHE IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The purpose of the present invention is exactly in order to overcome the shortcoming that Grignard reagent synthetic reaction solvent exists in the prior art or production cost is high, technical process is difficult to control, or product toxicity is bigger, and proposes a kind of new Grignard for above-mentioned shortcoming Reagent Synthesis Reaction Solvent

Method used

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  • Grignard reagent synthesis reaction solvent in maltol production
  • Grignard reagent synthesis reaction solvent in maltol production
  • Grignard reagent synthesis reaction solvent in maltol production

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1: throw 60Kg of magnesium chips in the Grignard reactor, add cyclohexane and tetrahydrofuran solvent (3: 1) 1200L prepared (hexanaphthene and tetrahydrofuran directly mix and stir and get final product), logical chloromethane reacts, then with After furfural addition and hydrolysis reaction, solid-liquid separation, vacuum distillation, 250Kg of intermediate product furfuryl alcohol was obtained, and the quality of chromatographic analysis was qualified. Cyclohexane and tetrahydrofuran are distilled out, collected by brine condensation, dried and dehydrated with anhydrous calcium chloride, and recycled.

Embodiment 2- Embodiment 4

[0020] Embodiment 2-embodiment 4, basic process is the same as embodiment 1, just the ratio of cyclohexane and tetrahydrofuran solvent is different, see the table below.

[0021] Example

[0022] Effect: From application examples 1 to 4, after using the mixture of cyclohexane and tetrahydrofuran as the Grignard synthesis reaction solvent, the quantity and quality of the intermediate product produced is stable, fully meeting the production requirements of the subsequent process; production consumption and cost are reduced; and avoid The highly toxic chemical pure benzene is used to improve the production and operation environment; at the same time, it meets the food safety requirements of domestic and foreign users.

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Abstract

The invention relates to a Grignard reagent synthesis solvent used in the production of maltol. The solvent is characterized in that the solvent is mixed by the raw material with the mixture ratio of: 2.6-3.2 of cyclohexane, 0.8-1.2 of tetrahydrofuran. The invention has the advantages that: cyclohexane is of little toxicity and is an allowed solvent listed in the safe foodstuffs by the European Union and U.S standards; experiment and application show that no change to the production equipment is made, only replacing the solvent and having a proper adjustment to the process index; the production operation is normal, the reaction can be easily controlled and the production cost is low.

Description

Technical field: [0001] The invention relates to a reaction solvent used in the production of spice maltol (including ethyl maltol), in particular to a Grignard reagent synthesis reaction solvent therein. Background technique: [0002] Maltol (and ethyl maltol) is a broad-spectrum flavor enhancer with a pleasant burnt-sweet aroma, widely used in daily chemical, beverage, food, medicine, tobacco, wine and other fine chemical fields. At present, the production process of maltol (and ethyl maltol) mainly adopts the furfural route. The production process is: the reaction of magnesium and alkyl halides in the presence of anhydrous ether or tetrahydrofuran solvents to synthesize Grignard reagents, and then Grignard reagents and furfural addition reaction , and then hydrolyzed to obtain the furfuryl alcohol intermediate; the furfuryl alcohol intermediate after the separation of the solvent was chlorinated with chlorine gas at a low temperature in methanol aqueous solution, and then...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D309/40C07B49/00
Inventor 杨迎春
Owner ANHUI JINGHE IND
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