Method for synthesizing L-ascorbyl palmitate

Abstract

The invention discloses a method for synthesizing L-ascorbyl palmitate, which comprises the following steps: grinding L-ascorbyl palmitate into fine powder; at 25 to 20 DEG C, slowly adding the L-ascorbyl palmitate fine powder into pure sulfuric acid so that the L-ascorbyl palmitate fine powder dissolves in the sulfuric acid; adding L-ascorbyl palmitate in an amount which is 0.95 times the molar number of L-ascorbyl palmitate into the reaction solution, adding dehydrating agent into the reaction solution, and continuing reaction for 6 to 7 hours; pouring the generated reaction solution into broken ice, filtering out coarse product, drying and washing with water; heating the prepared coarse L-ascorbyl palmitate, dissolving the coarse L-ascorbyl palmitate in ethyl acetate, and decolorizing and purifying the solution by particle active carbon; and subjecting the obtained solution to reduced-pressure distillation and concentration, cooling feed liquid to 0 DEG C and discharging to obtain L-ascorbyl palmitate white powder. When the method disclosed by the invention is used, the production efficiency can be improved greatly, the production period is shortened, the product yield is increased, the product quality is improved, and the dose of palmitic acid is reduced (only 5 percent more is required).

Description

technical field

[0001] The present invention relates to the synthetic method of organic compound, specifically a kind of synthetic method of L-ascorbyl palmitate. Background technique

[0002] With the development of the economy and the improvement of living standards, people have higher and higher requirements for the quality of oil and oily food. Using antioxidants to delay the oxidation of fats and oily foods is the most effective means of storing fats and oily foods. L-ascorbyl palmitate is a new, fat-soluble, non-toxic and harmless multifunctional nutritional antioxidant received widespread attention. L-ascorbyl palmitate is also a new type of food additive recognized internationally in recent years, so it is widely used in grain, oil, food, medicine, health care products, cosmetics and other fields.

[0003] L-ascorbyl palmitate is L-ascorbyl-6-palmitate, abbreviation: L-AP or AP; English name: L-ascorbyl palmitate; molecular formula: C 22 h 38 o 7 , Molecular wei...

Examples

Embodiment 1

[0019] a. Crush palmitic acid into 100-mesh fine powder; b. Slowly add 250 grams of palmitic acid fine powder into a reaction bottle containing 1000 ml of pure sulfuric acid at 25°C to dissolve for 1 hour; c. Add 163.03 grams to the reaction solution After 3 hours of L-ascorbic esterification reaction, add 0.46 moles of sulfur trioxide to the reaction solution, and continue the esterification for 7 hours (the process of this step uses a dehydrating agent to react the water generated by the reaction in the middle of the reaction, which promotes the esterification process. The reaction proceeds in the forward direction, which not only reduces the amount of palmitic acid, simplifies the purification process, but also improves the yield of the synthesis reaction.); d, the reaction is completed, the reaction solution is poured into crushed ice, and a large amount of white solid is precipitated , filtered to obtain the crude product of L-ascorbyl palmitate, and the filter cake was va...

Embodiment 2

[0021] (1) At 25°C, slowly add 250 grams of 120-mesh palmitic acid fine powder into a reaction bottle containing 1000 ml of 98.3% sulfuric acid to dissolve for 1 hour; (2) Add 163.03 grams of L-ascorbic acid to the reaction solution to react After 2 hours, add 0.46 moles of sulfur trioxide to the reaction solution, and continue the esterification for 6 hours; (3) After the reaction is completed, the reaction solution is poured into crushed ice, and a large amount of white solid is precipitated, which is filtered to obtain L-ascorbyl palmitate For the crude acid ester, the filter cake was vacuum-dried at 28°C and washed with pure water until neutral; (4) The crude L-ascorbyl palmitate was heated and dissolved in 3840ml of ethyl acetate, and then the solution was decolorized through a granular activated carbon column, Impurity removal and purification; (5) passing the filtrate through a drying column filled with 3A molecular sieve adsorbent to remove trace moisture in the filtra...

Embodiment 3

[0023] (1) At 25°C, slowly add 250 grams of 160-mesh palmitic acid fine powder into a reaction flask filled with 1000ml of 100% concentrated sulfuric acid to dissolve for 1 hour; (2) Add 163.03 grams of L-ascorbic acid to the reaction solution and react for 3 hours , and then add 0.46 moles of sulfur trioxide to the reaction solution, and continue the esterification for 7 hours; (3) After the reaction is completed, the reaction solution is poured into crushed ice, and a large amount of white solid is precipitated, which is filtered to obtain the crude product of L-ascorbyl palmitate , the filter cake was vacuum-dried at 30°C and washed with pure water until neutral; (4) The crude product of L-ascorbyl palmitate was heated and dissolved in 3840ml of ethyl acetate, and then the solution was passed through a granular activated carbon column for decolorization, impurity removal, Purification; (5) Distill the filtrate under reduced pressure, concentrate and crystallize, and cool the...

technical field

[0001] The present invention relates to the synthetic method of organic compound, specifically a kind of synthetic method of L-ascorbyl palmitate. Background technique

[0002] With the development of the economy and the improvement of living standards, people have higher and higher requirements for the quality of oil and oily food. Using antioxidants to delay the oxidation of fats and oily foods is the most effective means of storing fats and oily foods. L-ascorbyl palmitate is a new, fat-soluble, non-toxic and harmless multifunctional nutritional antioxidant received widespread attention. L-ascorbyl palmitate is also a new type of food additive recognized internationally in recent years, so it is widely used in grain, oil, food, medicine, health care products, cosmetics and other fields.

[0003] L-ascorbyl palmitate is L-ascorbyl-6-palmitate, abbreviation: L-AP or AP; English name: L-ascorbyl palmitate; molecular formula: C 22 h 38 o 7 , Molecular wei...

Examples

Embodiment 1

[0019] a. Crush palmitic acid into 100-mesh fine powder; b. Slowly add 250 grams of palmitic acid fine powder into a reaction bottle containing 1000 ml of pure sulfuric acid at 25°C to dissolve for 1 hour; c. Add 163.03 grams to the reaction solution After 3 hours of L-ascorbic esterification reaction, add 0.46 moles of sulfur trioxide to the reaction solution, and continue the esterification for 7 hours (the process of this step uses a dehydrating agent to react the water generated by the reaction in the middle of the reaction, which promotes the esterification process. The reaction proceeds in the forward direction, which not only reduces the amount of palmitic acid, simplifies the purification process, but also improves the yield of the synthesis reaction.); d, the reaction is completed, the reaction solution is poured into crushed ice, and a large amount of white solid is precipitated , filtered to obtain the crude product of L-ascorbyl palmitate, and the filter cake was va...

Embodiment 2

[0021] (1) At 25°C, slowly add 250 grams of 120-mesh palmitic acid fine powder into a reaction bottle containing 1000 ml of 98.3% sulfuric acid to dissolve for 1 hour; (2) Add 163.03 grams of L-ascorbic acid to the reaction solution to react After 2 hours, add 0.46 moles of sulfur trioxide to the reaction solution, and continue the esterification for 6 hours; (3) After the reaction is completed, the reaction solution is poured into crushed ice, and a large amount of white solid is precipitated, which is filtered to obtain L-ascorbyl palmitate For the crude acid ester, the filter cake was vacuum-dried at 28°C and washed with pure water until neutral; (4) The crude L-ascorbyl palmitate was heated and dissolved in 3840ml of ethyl acetate, and then the solution was decolorized through a granular activated carbon column, Impurity removal and purification; (5) passing the filtrate through a drying column filled with 3A molecular sieve adsorbent to remove trace moisture in the filtra...

Embodiment 3

[0023] (1) At 25°C, slowly add 250 grams of 160-mesh palmitic acid fine powder into a reaction flask filled with 1000ml of 100% concentrated sulfuric acid to dissolve for 1 hour; (2) Add 163.03 grams of L-ascorbic acid to the reaction solution and react for 3 hours , and then add 0.46 moles of sulfur trioxide to the reaction solution, and continue the esterification for 7 hours; (3) After the reaction is completed, the reaction solution is poured into crushed ice, and a large amount of white solid is precipitated, which is filtered to obtain the crude product of L-ascorbyl palmitate , the filter cake was vacuum-dried at 30°C and washed with pure water until neutral; (4) The crude product of L-ascorbyl palmitate was heated and dissolved in 3840ml of ethyl acetate, and then the solution was passed through a granular activated carbon column for decolorization, impurity removal, Purification; (5) Distill the filtrate under reduced pressure, concentrate and crystallize, and cool the...