A kind of riboflavin sodium phosphate compound injection and preparation method thereof
A technology for riboflavin sodium phosphate and compound, applied in the field of riboflavin sodium phosphate compound injection and preparation thereof, can solve the problems of low yield of riboflavin sodium phosphate, difficult reaction control, many reaction by-products and the like, and achieves The effect of shortening reaction time, stable properties and uniform particle size
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Embodiment 1
[0023] Embodiment 1: a kind of riboflavin sodium phosphate compound, its preparation method is as follows:
[0024] Riboflavin pretreatment: add riboflavin to the mixed acid solution, the mass of the mixed acid solution is 8 times the mass of riboflavin, the mass composition of the mixed acid is acetic acid: lactic acid = 4:1, and then heated to 85°C , keep the temperature for 2 hours and then raise the temperature to 145° C., remove the mixed acid, and dry to obtain the pretreated riboflavin.
[0025] Add 25 g of pretreated riboflavin, 8 ml of distilled water and phosphorus oxychloride in sequence to 100 ml of acetonitrile, stir well and react at 35 °C for 33 min; then add 80 ml of distilled water, raise the temperature to 60 °C for 2 h, then cool down to room temperature , filter to remove the insoluble matter in the reaction solution, add sodium hydroxide to the filtrate to adjust the pH to 5.8, stir and react at room temperature for 18 min, filter, wash the filter cake wit...
Embodiment 2
[0033] Embodiment 2: a kind of riboflavin sodium phosphate compound, its preparation method is as follows:
[0034] Riboflavin pretreatment: add riboflavin to the mixed acid solution, the mass of the mixed acid solution is 6 times the mass of riboflavin, the mass composition of the mixed acid is acetic acid: lactic acid = 3:1, and then heated to 80°C , keep the temperature for 1 hour and then raise the temperature to 140° C., remove the mixed acid, and dry to obtain the pretreated riboflavin.
[0035] Add 20g of pretreated riboflavin, 3ml of distilled water and phosphorus oxychloride to 100ml of acetonitrile in sequence, stir well and react at 30°C for 30min; then add 70ml of distilled water, raise the temperature to 60°C for 2h, then cool down to room temperature, Remove the insoluble matter in the reaction solution by filtration, add sodium hydroxide to the filtrate to adjust the pH to 5.5, stir and react at room temperature for 15 min, filter, wash the filter cake with 50% ...
Embodiment 3
[0038] Embodiment 3: a kind of riboflavin sodium phosphate compound, its preparation method is as follows:
[0039] Riboflavin pretreatment: add riboflavin to the mixed acid solution, the mass of the mixed acid solution is 10 times the mass of riboflavin, the mass composition of the mixed acid is acetic acid: lactic acid = 6:1, and then heated to 90°C , keep the temperature for 3 hours and then raise the temperature to 150° C., remove the mixed acid, and dry to obtain the pretreated riboflavin.
[0040] Add 30 g of pretreated riboflavin, 10 ml of distilled water and phosphorus oxychloride in sequence to 100 ml of acetonitrile, stir well and react at 40 °C for 35 min; then add 90 ml of distilled water, heat up to 60 °C for 2 h, then cool down to room temperature , filtered to remove the insoluble matter in the reaction solution, added sodium hydroxide to the filtrate to adjust the pH to 6.1, stirred at room temperature for 20 min, filtered, washed the filter cake with a 50% eth...
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