A method for preparing folic acid
A folic acid and sulfate technology, applied in the field of medicine, can solve the problems of increasing labor intensity and production cost, cumbersome refining process, low total yield, etc., and achieves the effects of short reaction time, avoiding a large amount of waste water and high product purity
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Embodiment 1
[0024] Feeding ratio:
[0025]
[0026] Steps:
[0027] Add 100g N-p-aminobenzoyl glutamic acid, 120g 2,4,5-triamino-6-hydroxypyrimidine sulfate in the reaction flask, 160g 1,1,3-trichloroacetone, 140g sodium metabisulfite, 100g 1 -Ethyl-3-methylimidazolium tetrafluoroborate ([emim]BF4), stirring and controlling the temperature at 20-30°C for 2 hours. During the reaction, use sodium hydroxide to adjust the pH value of the system to 3.0-3.5, and stop after the reaction Stir and filter to obtain crude folic acid.
[0028] Add the obtained folic acid crude product and 4.5L purified water into the reaction flask, heat to 80-90°C under stirring, then adjust the pH of the system to 8-9 with sodium hydroxide solution (2N), add 15g of activated carbon and keep stirring for 30 minutes to decolorize , hot filter. Control the temperature of the filtrate at 80-90°C, add dilute hydrochloric acid (2N) to adjust the pH to 3.0-3.5, slowly cool down to room temperature, filter, put the f...
Embodiment 2
[0030] Feeding ratio:
[0031]
[0032] Steps:
[0033] Add 100g N-p-aminobenzoyl glutamic acid, 120g 2,4,5-triamino-6-hydroxypyrimidine sulfate in the reaction flask, 160g 1,1,3-trichloroacetone, 140g sodium metabisulfite, 150g 1 -Butyl-3-methylimidazolium hexafluorophosphate ([bmim]PF6), stirring and controlling the temperature at 30-40°C for 1h30min, during the reaction, use potassium hydroxide to adjust the pH value of the system to 4.0-5.0, and stop stirring after the reaction , filtered to obtain crude folic acid.
[0034] Add the obtained folic acid crude product and 4.5L of purified water into the reaction flask, heat to 80-90°C under stirring, then adjust the pH of the system to 8-9 with potassium hydroxide solution (2N), add 15g of activated carbon and keep stirring for 30 minutes to decolorize , hot filter. Control the temperature of the filtrate at 80-90°C, add dilute hydrochloric acid (2N) to adjust the pH to 3.0-3.5, slowly cool down to room temperature, fi...
Embodiment 3
[0036] Feeding ratio:
[0037]
[0038] Steps:
[0039] Add 100g N-p-aminobenzoyl glutamic acid, 160g 2,4,5-triamino-6-hydroxypyrimidine sulfate in the reaction flask, 150g 1,1,3-trichloroacetone, 150g sodium metabisulfite, 80g N -Butylpyridine hexafluorophosphate (BPyPF6), stirring and controlling the temperature at 40-50°C for 2h15min, during the reaction, adjust the pH of the system to 2.0-3.0 with sodium hydroxide, stop stirring after the reaction, and filter to obtain crude folic acid.
[0040] Add the obtained folic acid crude product and 4.5L of purified water into the reaction flask, heat to 80-90°C under stirring, then adjust the pH of the system to 8-9 with sodium carbonate solution (1N), add 15g of activated carbon and keep stirring to decolorize for 30 minutes. hot filter. Control the temperature of the filtrate at 80-90°C, add dilute hydrochloric acid (2N) to adjust the pH to 3.0-3.5, slowly cool down to room temperature, filter, put the filter cake in an ove...
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