Solvent-free method for synthesizing water-soluble vitamin E polyethylene glycol succinic acid ester
A technology of polyethylene glycol succinate and water-soluble vitamins, applied in the direction of organic chemistry, can solve problems affecting mass transfer and reaction rate, adverse effects on safety, and complicated separation process, so as to reduce recovery and rectification, The effect of no solvent consumption and simple subsequent separation
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Embodiment 1
[0022] Take by weighing 5.6 gram purity to be the natural vitamin E succinate of 90%, 20 gram molecular weight is the polyethylene glycol 600 of 600, 0.8 gram mass percent concentration is the concentrated sulfuric acid of 98%, put into three-necked bottle, in 100 The reaction was stirred at constant temperature at ℃ for 2 hours, and cooled to room temperature after the reaction was completed. The reaction product was transferred to a round-bottomed flask, and then 150 ml of ethyl acetate was added to the round-bottomed flask to obtain a mixture. The mixture was transferred to a separatory funnel, extracted three times with saturated brine, and the organic phase was collected. The organic phase was evaporated to remove the solvent to obtain 8.3 grams of TPGS. The purity of the product obtained by HPLC was 90.1%, the conversion rate of vitamin E succinate was 89.2%, and the yield of TPGS was 79.2%.
Embodiment 2
[0024] Take by weighing 5.3 grams of natural vitamin E succinates with a purity of 95%, 20 grams of polyethylene glycol 1200 with a molecular weight of 1200, and 1.5 grams of concentrated hydrochloric acid with a concentration of 36% in a three-necked bottle. The reaction was stirred at constant temperature at ℃ for 3 hours, and cooled to room temperature after the reaction was completed. The reaction product was transferred to a round-bottomed flask, and then 150 ml of ethyl acetate was added to the round-bottomed flask to obtain a mixture. The mixture was transferred to a separatory funnel, extracted three times with saturated brine, and the organic phase was collected. The organic phase was evaporated to remove the solvent to obtain 13.5 grams of TPGS. The purity of the product obtained by HPLC was 93.5%, the conversion rate of vitamin E succinate was 92.7%, and the yield of TPGS was 83.7%.
Embodiment 3
[0026] Weigh 5.6 grams of synthetic vitamin E succinate with a purity of 85%, 35 grams of polyethylene glycol 800 with a molecular weight of 800, and 3.8 grams of p-toluenesulfonic acid, put them in a three-necked bottle, and stir at 110 ° C for reaction 4 hours, and cooled to room temperature after the reaction. The reaction mixture was transferred to a round-bottomed flask, and then 150 ml of ethyl acetate was added to the round-bottomed flask to obtain a mixture. The mixture was transferred to a separatory funnel, extracted three times with saturated brine, and the organic phase was collected. The organic phase was evaporated to remove the solvent to obtain 9.6 grams of TPGS. The purity of the product obtained by HPLC was 92.0%, the conversion rate of vitamin E succinate was 90.3%, and the yield of TPGS was 82.9%.
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