Methane → HCID 57295602, compound

Participants

Reaction Steps

100.2 g of acetic anhydride was added to 61.0 g of (4S,5S)-4,5-bis(acetoxymethyl)-1,3-dioxolane obtained in Example 15. To this was added 11.8 g of glacial acetic acid to dissolve the mixture. 3.4 g of anhydrous zinc chloride was added while stirring. The zinc chloride was slowly dissolved to change the color of the mixture from yellow into charcoal. After the reaction overnight, the reaction mixture was charged into a separating funnel which contained 500 ml of ethyl acetate. To this was added saturated aqueous solution of sodium hydrogen carbonate to neutralize. After washing with water and drying, the product was concentrated by evaporator. Acetic anhydride not decomposed was removed by a chemical pump to obtain 91.9 g (yield: 87.7%) of an yellow oil of the title compound.

Provenance & Evidence