In a 500 mL round bottom flask add 10 g glucose, acetic acid 100 mL, acetic anhydride 32.5 mL, p-toluenesulfonic acid 0.5 g, ultrasonic reaction for 10 minutes, the above reaction solution add acetyl bromide 12.5 mL, methanol 9.0 mL, ultrasonic vibration, power 420W (model DST20500) reaction for 1 hour, TLC detection of the reaction is complete, add Dichloromethane was diluted, washed with water and recrystallized with ethanol to obtain 21.9 g of bromoglucose crystals with 96% yield.
In the above bromodextrose add -cyclodextrin 44 g, 220 mL of water and 11 g of zinc powder, ultrasonic power 480W, (model DST20500) oscillation reaction for 10 minutes, add ethyl acetate dilution, filtration, filtrate extracted with ethyl acetate for 3 times, combined with the organic phase, add anhydrous sodium sulfate drying, filtration, concentration under reduced pressure, the crude acetylated glucosinolates, and then recrystallized with ethyl acetate and petroleum ether to get acetylated glucose, and then recrystallized with ethanol and petroleum ether to get acetylated glucosinolates. And then recrystallized with ethyl acetate and petroleum ether to get acetylated glucosinolates pure product 13.8 g, the yield is 95%.
