Method for synthesizing L-ascorbyl palmitate
A technology of ascorbyl palmitate and synthesis method, which is applied in the direction of organic chemistry, can solve the problems of increasing the difficulty of purification steps, affecting product quality, and difficulty in acid washing process, so as to avoid emulsification of crude products, solve long reaction time, and simplify purification process Effect
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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...
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