Sulfuric Acid → HCID 67042319, compound

Participants

Reaction Steps

138.63 g of the mixture from step 3 were dissolved in 1.4 l of ethanol and 60 ml of concentrated sulfuric acid and the solution was boiled at reflux for 25 h. Then 1.3 l of ethanol were removed on a rotary evaporator and the residue was admixed with 1 l of ice-water, rendered basic using saturated NaHCO3 solution, and then extracted with three times 500 ml of dichloromethane. The combined organic phases were dried over MgSO4, filtered with suction over silica gel, and concentrated. The product was then subjected to chromatographic separation (silica gel, heptane/ethyl acetate 9:1).

Provenance & Evidence