Preparation method for acetyl-L-carnitine nitrate
A technology of acetyl-L-carnitine and L-carnitine, applied in the field of preparation of acetyl-L-carnitine nitrate, can solve problems such as enhancement, and achieve the effects of reducing waste, facilitating purification and high yield
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[0028] ⅰ. Preparation of acetyl-L-carnitine:
[0029] a. Adding L-carnitine in the reaction vessel is a raw material, adding acetic acid is a solvent, and L-carnitine is dissolved;
[0030] b. Then add acetic anhydride and react at 30°C~80°C for 3~12 hours;
[0031] c. After the reaction is completed, distill under reduced pressure to remove the acetic acid in the solution, then add acetone to fully stir and disperse;
[0032] d. Cool down to below 5°C to crystallize, and keep warm at 0°C~5°C for more than 2 hours;
[0033] e. Suction filtration to separate the solid, and drying to obtain acetyl-L-carnitine;
[0034] ⅱ. Preparation of acetyl-L-carnitine nitrate:
[0035] a. taking the acetyl-L-carnitine gained in step i as a raw material, adding acetic acid as a solvent, and dissolving the acetyl-L-carnitine;
[0036] b. Then add nitric acid and react at 30°C~80°C for 2~5 hours;
[0037] c. After the reaction is completed, distill the acetic acid and water in the solution...
Embodiment 1
[0047] Add 96g of acetic acid into the reaction vessel, and add 32g of L-carnitine to dissolve under stirring. After completely dissolving, add 61.5g of acetic anhydride, then raise the temperature to 80°C and react at a constant temperature for 12 hours. Distill acetic acid below ℃, lower the temperature to 40℃, add 160g of acetone, fully stir and disperse for 0.5 hours, cool down to below 5℃ to crystallize, and keep warm for 2 hours between 0℃~5℃, separate by suction filtration, and wash the solid with acetone , dried in vacuum -0.09 Mpa, 80°C, and obtained 36g of finished product of acetyl-L-carnitine, with a yield of 88.9%.
[0048] Take 20.5g of the finished product of acetyl-L-carnitine and put it into the reaction container, then add 62g of acetic acid, stir to dissolve, raise the temperature to 60°C, add 14.5g of nitric acid, then raise the temperature to 80°C and react at constant temperature for 5 hours. , the temperature is below 80°C to distill off acetic acid, low...
Embodiment 2
[0050] Add 200g of acetic acid into the reaction vessel, and add 130g of L-carnitine under stirring to dissolve. After it is completely dissolved, add 166g of acetic anhydride, then raise the temperature to 30°C and react at a constant temperature for 3 hours. Remove acetic acid by distillation, lower the temperature to 40°C, add 260g of acetone, fully stir and disperse for 0.5 hours, cool down to below 5°C to crystallize, and keep warm at 0°C~5°C for 2 hours, separate by suction filtration, wash the solid with acetone, Dry at -0.09 Mpa in a vacuum at 80°C to obtain 147g of the finished product of acetyl-L-carnitine, with a yield of 89.2%.
[0051] Take 147g of the finished product of acetyl-L-carnitine and put it into the reaction container, then add 220g of acetic acid, stir to dissolve, raise the temperature to 30°C, add 105g of nitric acid, and then react at a constant temperature of 30°C for 2 hours. Distill and remove acetic acid at ℃, add 294g of acetone to fully stir a...
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