A kind of refining method of troxerutin
A refining method and crude product technology, applied in chemical instruments and methods, preparation of sugar derivatives, organic chemistry, etc., can solve the problems of unqualified solubility, low purity of Troxerutin, etc., and achieve strong repeatability, simple operation and process. simple effect
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Embodiment 1
[0016] A method for refining troxerutin, the process is as follows:
[0017] Add 30g of troxerutin crude product with a purity of 88% to the reaction flask, add 30g of purified water, raise the temperature to 65-68°C, add 6g of impurity remover EDTA, add 0.3g of activated carbon after the solution is clarified, and stir at 90-95°C for 30 minutes. Filter while it is hot, transfer the filtrate to the dropping funnel, and set aside; put another 160g of methanol in a three-necked flask, and slowly add the filtrate dropwise under stirring. 0~5℃), and dried at 70~80℃ to obtain pure troxerutin, with a weight yield of 78.3% and a purity of 98.3%. The impurity-removing agent A was not detected in the pure troxerutin, which met the requirements for medicinal use.
Embodiment 2
[0019] A method for refining troxerutin, the process is as follows:
[0020] Add 30g of crude troxerutin with a purity of 85% to the reaction flask, add 36g of purified water, raise the temperature to 65-68°C, add 9g of impurity remover A EDTA sodium, add 0.2g of activated carbon after the solution is clarified, and stir at 90-95°C for 30 minutes, filter while hot, transfer the filtrate to the dropping funnel, and set aside; another 450g of ethanol is placed in a three-necked flask, and slowly add the filtrate dropwise under stirring. Washing with methanol (0-5°C) and drying at 70-80°C gave pure troxerutin, with a weight yield of 71.8% and a purity of 98.8%. The impurity remover A was not detected in the pure troxerutin, which met the requirements for medicinal use.
Embodiment 3
[0022] A method for refining troxerutin, the process is as follows:
[0023] Add 30g of crude troxerutin with a purity of 83% to the reaction flask, add 39g of purified water, raise the temperature to 65-68°C, add 8g of impurity remover A EDTA, add 0.15g of activated carbon after the solution is clarified, and stir at 90-95°C for 30 minutes , filtered while hot, and the filtrate was transferred to a dropping funnel for use; another 200g of methanol and 200g of isopropanol were placed in a three-necked flask, and the filtrate was slowly added dropwise under stirring. The cake was washed with 30g of ice methanol (0-5°C), and dried at 70-80°C to obtain pure troxerutin, with a weight yield of 75.4% and a purity of 98.5%. The impurity remover A was not detected in the pure troxerutin, which met the requirements of Medicinal requirements.
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