Anthrax capsule surface carbohydrate antigen-based novel trisaccharide 4-methoxyphenoside compound and preparation method thereof
A technology for methoxyphenol glycosides and compounds, which is applied in the field of oligosaccharide synthesis, can solve the problems of unclear antigen, uncertainty, complex composition and the like, and achieves the effects of simple synthesis route, good stereoselectivity and low cost of raw materials
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[0036] (1) Preparation of monosaccharide acceptor (6)
[0037] Commercially available glucosamine hydrochloride 1 (40 g, 186 mmol) and sodium bicarbonate (46.8 g, 558 mmol) were dissolved in 360 mL of distilled water. After the reaction was stirred at room temperature for 30 min, 2,2,2-trichloroethyl chloroformate (Troc-Cl, 30 mL, 233 mmol) was slowly added, and the reaction was continued to stir for 4 h. The solvent was removed by filtration and dried to give a pale yellow residue (54 g, 150 mmol). Dissolve in 200mL of pyridine, and slowly add acetic anhydride (88mL, 900mmol) dropwise in ice bath. The reaction solution was stirred overnight at room temperature. After TLC detected that the reaction was complete, 100 mL of methanol was added to quench the reaction. The solvent was pulled dry, extracted with 500 mL of ethyl acetate, and then washed with saturated sodium bicarbonate solution, 1M hydrochloric acid solution and saturated sodium chloride solution in sequence. Th...
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