Biphenyl ammonia acetate butantriol salt and preparation method thereof
A technology of felbinac tromethamine and phenylacetic acid tromethamine salt, which is applied in the field of felbinac tromethamine salt compound and its preparation, and can solve the problems that it can only be used as an external drug and affects the popularization and use of drugs. , to achieve the effect of simple and feasible synthesis process, reasonable design and easy access to raw materials
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Embodiment 1
[0021] Embodiment 1: the preparation of felbinac tromethamine salt
[0022] In a dry and clean 250ml three-neck round bottom flask, add 21.2g (0.1mol) of felbinac and 210ml of methanol, heat to 60°C and stir until completely dissolved, then add 12.1g (0.1mol) of tromethamine at 60°C, and mix The solution was clear and transparent, stirred and reacted under this condition for 1 hour, and TLC detected that the reaction was complete. After cooling below 0°C for 5 hours, a large amount of white crystals precipitated, which were filtered by suction and vacuum-dried at 80°C to obtain 30.5 g of white crystalline felbinac tromethamine salt. Measured: mp: 162-163°C, yield 91.6%. The product is analyzed by elements (theoretical value: C64.9% H6.9% N4.2% O24%;
[0023] Measured value: C64.1% H7.3% N3.6% O25%), NMR, MS, UV, IR and HPLC analysis, the product is felbinac tromethamine salt, the purity is 99.5%.
[0024] Determination of felbinac tromethamine sample solubility:
[0025] A...
Embodiment 2
[0031] Embodiment 2: the preparation of felbinac tromethamine salt
[0032] In a dry and clean 250ml single-necked round bottom flask, add 21.2g (0.1mol) felbinac and 12.1g (0.1mol) tromethamine, add 150ml absolute ethanol to it, shake and heat to completely dissolve until clear , keep the temperature (50° C.) for 30 min, and concentrate to dryness under reduced pressure with a rotary evaporator to obtain a white powder. Dry in vacuum at 80°C to obtain 32.0 g of felbinac tromethamine salt. mp: 163-164°C, yield: 96.0%, the product is analyzed by elemental analysis, NMR, MS, IR, UV and high performance liquid chromatography, and the product is felbinac tromethamine salt with a purity of 99.2%.
Embodiment 3
[0033] Embodiment 3: the preparation of felbinac tromethamine
[0034] In a dry and clean 250ml three-necked round-bottomed flask, add 21.2g (0.1mol) felbinac and 200ml benzene, heat and stir until dissolved, then add 12.1g (0.1mol) tromethamine, mix until clear, The reaction was stirred at 70°C for 2 hours, and the end point of the reaction was identified by TLC. After the reaction was completed, a large amount of crystalline solid was precipitated by sufficient cooling, filtered by suction, washed with a small amount of anhydrous ether, and dried in a vacuum oven at 80°C to obtain 28.5 g of bismuth Tromethamine phenylacetate. mp: 163-164, yield 85.6%. The product is analyzed by elemental analysis, NMR, MS, IR, UV and HPLC. The product is felbinac tromethamine salt with a purity of 99.8%.
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