Method for preparing L-ascorbic acid-2-phosphate ester and salt
A technology of ascorbic acid and monophosphate, which is applied in the field of preparation of vitamin C derivatives, can solve the problems of loss of esterification activity, easy moisture absorption, stickiness, decomposition and destruction, etc., and achieve the effect of high content of L-ascorbic acid
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Embodiment 1
[0076] Preparation of L-ascorbic acid-2-monophosphate monosodium monocalcium salt
[0077]
[0078] Into a 250 ml flask equipped with a stirrer, a thermometer, an air duct, a pH meter electrode, and a dropping funnel, a nitrogen stream was introduced, 15 ml of water and 17.6 g (100 mmol) of L-ascorbic acid were added, stirred to dissolve, and the solution was cooled To below 0°C. Add 10 ml (100 mmol) of 10 mol / L sodium hydroxide solution dropwise while stirring. Control the temperature at -5°C±3°C, add 7.81 g (55 mmol) of phosphorus pentoxide and Calcium hydroxide 8.15 g (110 mmol) is prepared as a mixture, the molar ratio of L-ascorbic acid and phosphorus pentoxide is: 1:0.55, and the molar ratio of phosphorus pentoxide and calcium hydroxide is 1:2. About 2~3 After adding in 1 hour, keep the reaction at -5~0℃ for 2 hours, and react at 0~30℃ for 4 hours. Add concentrated sulfuric acid dropwise to pH 9, add 85ml of 95% ethanol, stir for 1 hour, filter, and dry to obtain off-...
Embodiment 2
[0081] Preparation of L-ascorbic acid-2-monophosphate disodium hemicalcium salt
[0082]
[0083] The reaction conditions are as example 1
[0084] Add 10 ml of water to 17.6 g (100 mmol) of L-ascorbic acid, stir to dissolve, and cool the solution to below 0°C. Add 10 milliliters (100 millimoles) of 10 mol / liter sodium hydroxide solution dropwise, add the mixture of 7.81 grams (55 millimoles) of phosphorus pentoxide and 4.08 grams (55 millimoles) of calcium hydroxide in stages, L- The molar ratio of ascorbic acid to phosphorus pentoxide is 1:0.55, and the molar ratio of phosphorus pentoxide to calcium hydroxide is 1:1. During the reaction, 10 mol / L sodium hydroxide solution was added dropwise to maintain pH 10-12. After the reaction, adjust the pH to 8.5-9 with sulfuric acid, add 80 ml of water to dilute, and then spray dry to obtain a light yellow powder product.
[0085] HPLC analysis measures, the L-ascorbic acid of 38.4% is L-ascorbic acid-2-monophosphate di-sodium h...
Embodiment 3
[0087] Preparation of L-ascorbic acid-2-monophosphate calcium salt
[0088]
[0089] The reaction conditions are as example 1
[0090]17.6 grams (100 millimoles) of L-ascorbic acid, add 20 milliliters of water, stir and dissolve, the solution is cooled to below 0 ℃. Add dropwise 18.5 grams (50 millimoles) of 20% (W / W) calcium hydroxide suspension, Add the mixture of phosphorus pentoxide 7.10 grams (50 mmol) and calcium hydroxide 7.41 grams (100 mmol) in stages, the molar ratio of L-ascorbic acid and phosphorus pentoxide is: 1: 0.5, phosphorus pentoxide The molar ratio to calcium hydroxide is 1:2. After the reaction, adjust the pH to 9 with sodium hydroxide solution and sulfuric acid, add 100 ml of 95% ethanol, stir for 0.5 hours, filter, and dry to obtain a white powder product.
[0091] HPLC analysis measures, the L-ascorbic acid of 36.2% is L-ascorbic acid-2-monophosphate calcium salt in the product, the L-ascorbic acid (L-ascorbic acid-2-dipolyphosphate salt, double L-a...
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