A kind of preparation method of fondaparinux sodium injection related substance b
A technology of fondaparinux sodium and related substances, which is applied in the field of medicine, can solve the problems of no literature reports on the synthesis method of substance B, and achieve the effects of easy large-scale preparation, high yield, and simple operation
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Embodiment 1
[0041]
[0042]Dissolve 25g of compound II, 15mL of pyridine, and 0.2g of 4-dimethylaminopyridine in 400mL of dichloromethane, add 11mL of benzoyl chloride dropwise in an ice-water bath, raise the temperature to room temperature for 10 hours, and add an appropriate amount of water to quench the reaction. Washed with 0.1M hydrochloric acid, water and saturated saline solution successively, dried over anhydrous sodium sulfate, filtered, spin-dried the solvent under reduced pressure, separated and purified by column to obtain 27 g of compound III as a white solid, with a yield of 95%.
Embodiment 2
[0044]
[0045] Dissolve 25g of compound III in a mixed solution of 25mL of dichloromethane and 250mL of 0.5M HCl / MeOH, stir at room temperature for 10h, filter under reduced pressure, wash the filter cake with water until neutral, and dry it with air at 50°C to obtain 18g of compound IV as a white solid , yield 80%.
Embodiment 3
[0047]
[0048] Take 15g compound IV, 38g SO 3 · NMe 3 , 15mL DMF and 150mL acetonitrile in a single-necked bottle, reacted at 50°C for 15h under nitrogen protection, cooled to 0°C, quenched by adding 40mL of methanol dropwise, and washed with saturated NaHCO 3 The pH of the aqueous solution was adjusted to 8, filtered, and concentrated under reduced pressure to remove the organic solvent to obtain an aqueous solution of the crude compound V, which was separated and purified on a C18 column to obtain 16 g of compound IV as a white solid, with a yield of 85%.
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