A kind of synthetic method of fudosteine
An addition reaction, cysteine technology, applied in the field of high-purity fodosteine synthesis, can solve the problems of complicated operation, long reaction time, increased cost, etc., and achieves simple process, mild and controllable reaction conditions, and low cost. low cost effect
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Embodiment 1
[0028] At 25-35°C, add L-cysteine (24.2g, 0.2mol) into a 250 mL four-neck flask, add 60 mL of water, add acetic acid dropwise under mechanical stirring, adjust pH=3.2, and react for 1 h Finally, acrolein (16.8g, 0.3mol) was added dropwise to the system. After dropping, reacted for 10 h, controlled in the liquid phase until the reaction was completed; at 15-25°C, added sodium borohydride (7.6g, 0.2mol) in the system, continue to stir for 2 h, adjust the pH=6 with NaOH solution, concentrate the solvent to obtain the crude product fudosteine; then add a certain proportion of ethanol aqueous solution 300 mL to the crude product, heat to 45°C to dissolve and stir for 30 min, then cooled and stirred at room temperature for 30 min and then filtered, the filter cake was rinsed with ethanol, and the filter cake was dried to obtain 34.3 g of refined fudosteine with a purity of 99.7% and a yield of 95.8%.
Embodiment 2
[0030] At 25-35°C, add L-cysteine (24.2g, 0.2mol) into a 250 mL four-neck flask, add 60 mL of water, add acetic acid dropwise under mechanical stirring, adjust pH=3.2, and react for 1 h Finally, acrolein (22.4g, 0.4mol) was added dropwise to the system. After dropping, reacted for 10 h, controlled in the liquid phase until the reaction was completed; at 15-25°C, added sodium borohydride (7.6g, 0.2mol) in the system, continue to stir for 2 h, adjust the pH=6 with NaOH solution, concentrate the solvent to obtain the crude product fudosteine; then add a certain proportion of ethanol aqueous solution 300 mL to the crude product, heat to 45°C to dissolve and stir for 30 min, then cooled and stirred at room temperature for 30 min and then filtered, the filter cake was rinsed with ethanol, and the filter cake was dried to obtain 33.8 g of refined fudosteine with a purity of 99.8% and a yield of 94.4%.
Embodiment 3
[0032] At 25-35°C, add L-cysteine (24.2g, 0.2mol) into a 250 mL four-neck flask, add 60 mL of water, add acetic acid dropwise under mechanical stirring, adjust pH=3.2, and react for 1 h Finally, acrolein (19.6g, 0.35mol) was added dropwise to the system. After dropping, reacted for 10 h, controlled in the liquid phase until the reaction was completed; at 15-25°C, added sodium borohydride (7.6g, 0.2mol) in the system, continue to stir for 2 h, adjust the pH=6 with NaOH solution, concentrate the solvent to obtain the crude product fudosteine; then add a certain proportion of ethanol aqueous solution 300 mL to the crude product, heat to 45°C to dissolve and stir for 30 min, then cooled and stirred at room temperature for 30 min and then filtered, the filter cake was rinsed with ethanol, and the filter cake was dried to obtain 34.5 g of refined fudosteine with a purity of 99.8% and a yield of 96.3%.
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