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L-ascorbyl palmitate and environment-friendly synthetic method thereof

A technology of ascorbyl palmitate and synthesis method, which is applied in the direction of organic chemistry, can solve the problems of high requirements for the reaction conditions of concentrated sulfuric acid, non-recyclable concentrated sulfuric acid, unfavorable environment, etc., and achieves low production cost, mild reaction conditions, and advanced technology. simple effect

Inactive Publication Date: 2014-04-23
东莞市感恩食品科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The existing method for synthesizing L-ascorbyl palmitate is generally to utilize liquid palmitic acid and L-ascorbic acid as raw materials, mix the raw materials in the presence of catalyst concentrated sulfuric acid, and directly carry out transesterification reaction to obtain L-ascorbyl palmitate , but in this synthesis method, the use of concentrated sulfuric acid not only has high requirements on the reaction vessel and reaction conditions, but also has great danger; in addition, concentrated sulfuric acid cannot be reused, resulting in a large amount of waste liquid discharge, which is unfavorable to the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A kind of synthetic method of L-ascorbyl palmitate, comprises the following steps:

[0023] a. Put 250g of palmitic acid into 1000g of N,N-dimethylformamide and stir until completely dissolved;

[0024] b. Put 250g of N,N-dicyclohexylcarbodiimide into the above reaction solution and stir continuously for 30min;

[0025] c. Put 150g of L-ascorbic acid into the above reaction solution, and continuously stir for 6 hours;

[0026] d. Put 130g of N-hydroxysuccinimide into the above reaction solution and stir continuously for 45min;

[0027] e. add 1500g water in above-mentioned reaction liquid and stir, filter and make crude product;

[0028] f. The prepared crude product was dissolved in ethyl acetate and recrystallized to obtain L-ascorbyl palmitate.

[0029] The yield of the L-ascorbyl palmitate of the present embodiment is 85%, and the purity is 98.5%.

Embodiment 2

[0031] A kind of synthetic method of L-ascorbyl palmitate, comprises the following steps:

[0032] a. Put 250g of palmitic acid into 750g of N,N-dimethylformamide and stir until completely dissolved;

[0033] b. Put 125g of N,N-dicyclohexylcarbodiimide into the above reaction solution and stir continuously for 20min;

[0034] c. Put 125g of L-ascorbic acid into the above reaction solution, and continuously stir for 1 hour;

[0035] d. Put 100g of N-hydroxysuccinimide into the above reaction solution and stir continuously for 30min;

[0036] e. add 1500g water in above-mentioned reaction liquid and stir, filter and make crude product;

[0037] f. the prepared crude product is dissolved in ethyl acetate and recrystallized to obtain L-ascorbyl palmitate;

[0038] g. The L-ascorbyl palmitate obtained in step f is subjected to centrifugal dehydration and vacuum drying.

[0039] The yield of the L-ascorbyl palmitate of the present embodiment is 86%, and the purity is 98%.

Embodiment 3

[0041] A kind of synthetic method of L-ascorbyl palmitate, comprises the following steps:

[0042] a. Put 250g of palmitic acid into 1250g of N,N-dimethylformamide and stir until completely dissolved;

[0043] b. Put 375g of N,N-dicyclohexylcarbodiimide into the above reaction solution and stir continuously for 40min;

[0044] c. Put 200g of L-ascorbic acid into the above reaction solution, and continuously stir for 10 hours;

[0045] d. Put 150g of N-hydroxysuccinimide into the above reaction solution and stir continuously for 60min;

[0046] e. add 1500g water in above-mentioned reaction liquid and stir, filter and make crude product;

[0047] f. the prepared crude product is dissolved in ethyl acetate and recrystallized to obtain L-ascorbyl palmitate;

[0048] g. The L-ascorbyl palmitate obtained in step f is subjected to centrifugal dehydration and vacuum drying.

[0049] The yield of the L-ascorbyl palmitate of the present embodiment is 86%, and the purity is 99%.

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Abstract

The invention relates to L-ascorbyl palmitate and an environment-friendly synthetic method thereof. The environment-friendly synthetic method comprises the following steps: dissolving palmitic acid and dicyclohexylcarbodiimide in N,N-dimethylformamide, adding L-ascorbic acid to perform esterification reaction; adding N-hydroxysuccinimide, stirring and filtering to obtain a crude product; dissolving the prepared crude product in ethyl acetate and performing recrystalization to obtain L-ascorbyl palmitate. The synthetic method of L-ascorbyl palmitate is simple in technology, does not need concentrated sulfuric acid as a catalyst during production, helps to substantially reduce requirements on reaction containers, reaction conditions and the like, is mild in reaction conditions and low in production cost, does not generate strong acid and other waste liquids discharge, and has no pollution to environment. Produced L-ascorbyl palmitate has the impurity up to 98% or more, has no mixed color and is high in quality.

Description

technical field [0001] The invention relates to the technical field of synthesis of fine chemicals, in particular to an L-ascorbyl palmitate and an environment-friendly synthesis method thereof. Background technique [0002] L-Ascorbyl palmitate is a new type, fat-soluble, non-toxic and harmless multifunctional nutritional antioxidant, which has strong antioxidant properties, and it can prevent the formation of free radicals and reduce fat when used in food It can effectively prevent the rancidity of fat and prolong the shelf life of oil and oily food. [0003] The existing method for synthesizing L-ascorbyl palmitate is generally to utilize liquid palmitic acid and L-ascorbic acid as raw materials, mix the raw materials in the presence of catalyst concentrated sulfuric acid, and directly carry out transesterification reaction to obtain L-ascorbyl palmitate , but in this synthesis method, the use of concentrated sulfuric acid not only has high requirements on the reaction v...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/62
CPCC07D307/62
Inventor 王力肖勇
Owner 东莞市感恩食品科技有限公司
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