The synthetic method of d-calcium pantothenate
A synthesis method and technology of calcium pantothenate are applied in the directions of organic chemistry methods, chemical instruments and methods, preparation of carboxylic acid amides, etc., and can solve the problems of high solvent consumption, high energy consumption, long time consumption, etc., and achieve complete conversion, high reaction efficiency, The effect of high product yield
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Embodiment 1
[0011] Embodiment 1: the synthesis of D-calcium pantothenate
[0012] (1) Add 650mL of anhydrous methanol to the reaction vessel, add 580g of D-pantolactone while stirring, then add 2g of activated carbon, stir for 0.5 hours, first coarsely filter, then finely filter, and retain the filtrate to obtain D-pantolide Hydrolyzed acid lactone methanol solution;
[0013] (2) Add 1800ml of anhydrous methanol to the reaction vessel, add 400g of beta-alanine while stirring, and then add 150g of calcium oxide, keep the reaction at 45°C for 2 hours, then add 5g of activated carbon, and stir for 0.5 hours. Filter, then precision filter, retain the filtrate, obtain β-alanine calcium methanol solution;
[0014] (3) the D-pantolactone methanol solution with a volume flow rate of 10ml / min and the β-alanine calcium methanol solution with a volume flow rate of 20ml / min are squeezed into the microchannel flow reactor (Corning Micro Channel reactor, G1 type), the reaction stays at 75-80°C for 15...
Embodiment 2
[0017] Embodiment 2: the synthesis of D-calcium pantothenate
[0018] According to the synthesis method of Example 1, the difference is that the reaction temperature in step (3) is 50-60°C.
[0019] Obtain 1062g white powder product by reaction, carry out physical and chemical detection to the product, the result is as follows: D-calcium pantothenate content is 89.0%, melting point 153-206.5 ℃, specific rotation [α]D 23 =+21.5°(C=1,H 2 O), the conversion rate of D-pantothenate lactone is 90%, and the D-calcium pantothenate productive rate is 89%.
Embodiment 3
[0020] Embodiment 3: the synthesis of D-calcium pantothenate
[0021] According to the synthesis method of Example 1, the difference is that the reaction temperature in step (3) is 100-120°C.
[0022] Obtain 1082g off-white powdery product by reaction, carry out physical and chemical detection to product, the result is as follows: D-calcium pantothenate content is 84.0%, fusing point 160-201.5 ℃, specific rotation [α]D 23 = +17.5°(C=1,H 2 O), the conversion rate of D-pantothenolactone is 100%, and the D-calcium pantothenate productive rate is 85%.
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