This invention discloses the preparation of
furan[3,4-d]-1,3,2-dioxathiol-4(3aH)-one, dihydro-,2-
oxide, comprising the following steps: 1. Dissolving D-isoascorbic acid in water and adding
sodium carbonate; 2. Adding 40 μL of 50% H2O2
aqueous solution dropwise. o C. Stir the reaction, then heat to 80°C. o C. Stir the reaction, filter while hot, wash with water to obtain a colorless and clear filtrate; 2. Quench the reaction with
hydrochloric acid dropwise to acidity, evaporate to
dryness under high vacuum to obtain a white
solid;
reflux with
ethyl acetate, filter, evaporate the filtrate by rotary
evaporation to obtain a crude intermediate, which is then processed to obtain a white needle-like crystalline intermediate; 3. Dissolve the white needle-like crystalline intermediate in
acetonitrile, add
thionyl chloride dropwise, and stir the reaction; 4. Pour the reaction solution into
ice water, extract with
dichloromethane, dry, filter, and evaporate by rotary
evaporation to obtain a yellow
solid crude product; further
processing yields the product. The advantages of this invention are: simple process
route, mild and easy-to-control reaction, low purification difficulty, few by-products, and high yield and purity.