A method for preparing troxerutin by self-priming stirring autoclave
An autoclave, self-priming technology, applied in the field of troxerutin synthesis, can solve the problems of reducing product yield, increasing production cost, increasing the difficulty of trihydroxyethylrutin, etc., and achieves improved purity and yield, The effect of reducing production cost and preventing leakage of ethylene oxide
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Embodiment 1
[0019] Weigh 30.53g (0.05mol) of rutin, 0.04g (0.25mmol) of catalyst natural weakly alkaline macromolecular compound chitosan, 100mL of solvent methanol and 11.0g (0.25mol) of ethylene oxide and add it to the self-priming stirring high pressure In the kettle, turn on the digital controller, set the temperature to 70°C, and the rotation speed to 1000r / min, stir to raise the temperature to 70°C, and keep the temperature for 6 hours. After the reaction, cool the cold water rapidly, stop stirring, turn off the digital controller, open the reaction kettle, pour out the reaction solution, adjust the pH of the poured out reaction solution to 5 with hydrochloric acid, and filter the catalyst. Seed crystals were added to the solution and allowed to stand for crystallization, and 33.79 g of crystals were obtained, with a yield of 91% and an external standard content of 88.3%.
Embodiment 2
[0021] Weigh 30.53g (0.05mol) of rutin, 2.42g (15mmol) of chitosan, a catalyst natural weakly alkaline macromolecular compound, 100mL of solvent methanol and 11.0g (0.25mol) of ethylene oxide into the self-priming stirring autoclave , turn on the digital controller, set the temperature to 75°C, and the rotation speed to 1000r / min, stir to raise the temperature to 75°C, and keep the temperature for 4h. After the reaction is over, cool down the cold water quickly, stop stirring, turn off the digital controller, open the reaction kettle, pour out the reaction solution, adjust the pH of the poured out reaction solution to 6 with hydrochloric acid, and filter the catalyst. Seed crystals were added to the liquid and allowed to stand for crystallization, and 35.28 g of crystals were obtained, with a yield of 95% and an external standard content of 89.7%.
Embodiment 3
[0023] Weigh 30.53g (0.05mol) of rutin, 0.04g (0.25mmol) of the catalyst natural weakly alkaline macromolecular compound chitosan, 100mL of solvent methanol and 15.4g (0.35mol) of ethylene oxide and add it to the self-priming stirring high pressure In the kettle, turn on the digital controller, set the temperature to 70°C, and the rotation speed to 1000r / min, stir to raise the temperature to 70°C, and keep the temperature for 5 hours. After the reaction is over, the cold water is cooled rapidly, and the stirring is stopped, the digital controller is turned off, the reaction kettle is opened, and the reaction liquid is poured out. The pH of the poured reaction solution was adjusted to 5.6 with hydrochloric acid, and the catalyst was suction-filtered. Seed crystals were added to the reaction solution after suction filtration and allowed to stand for crystallization. The crystals obtained were 34.16g, the yield was 92%, and the external standard content was 88.5 %.
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