A kind of preparation method of sugammadex sodium
A technology of sugammadex sodium and sodium ions, which is applied in the field of preparation of sugammadex sodium, and can solve the problems of long reaction route and cumbersome operation
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Embodiment 1
[0020] 2L three-neck flask, under nitrogen protection, add 1000ml of DMF and γ-cyclodextrin (100.0g 0.077mol), then add 3-mercaptopropionic acid (73.6g 0.694mol), cool down to -35°C, add trifluoromethane dropwise Sulfonic acid (98.4g 0.655mol), the temperature is controlled not to exceed -30°C, and the reaction is kept stirring for 3h. Add 5M aqueous sodium hydroxide solution dropwise to the reaction solution, adjust the pH to 9-10, heat up to 25°C and stir to react for 2 hours, suction filtration to obtain a solid, use DMF: water = 3:1 to beat for 2 hours, and filter to obtain smoother glucose Crude sodium product, yield: 70%, purity: 98%.
Embodiment 2
[0022] 2L three-neck flask, under nitrogen protection, add 1000ml of DMSO and γ-cyclodextrin (100.0g 0.077mol), then add 3-mercaptopropionic acid (73.6g 0.694mol), cool down to -35°C, add trifluoromethane dropwise Sulfonic acid (98.4g 0.655mol), the temperature is controlled not to exceed -30°C, and the reaction is kept stirring for 3h. 5M sodium methoxide aqueous solution was added dropwise to the reaction solution, adjusted to pH 9-10, the temperature was raised to 25°C and stirred for 2h, suction filtration to obtain a solid using DMF:water = 3:1, beating for 2h, and filtered to obtain sodium gluconate. Crude. Yield: 65%, Purity: 96%
Embodiment 3
[0024] 2L three-neck flask, under nitrogen protection, add 1000ml of formamide and γ-cyclodextrin (100.0g 0.077mol), then add 3-mercaptopropionic acid (73.6g 0.694mol), cool down to -35°C, add dropwise trifluoro Methanesulfonic acid (98.4g, 0.655mol), the temperature was controlled not to exceed -30°C, and the reaction was kept stirring for 3h. Add 5M aqueous sodium ethoxide solution dropwise to the reaction solution, adjust the pH to 9-10, heat up to 25°C and stir to react for 2 hours, suction filtration to obtain a solid, use DMF: water = 3:1 to beat for 2 hours, and filter to obtain sodium gluconate. Crude. Yield: 66%, Purity: 97%
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