Water → HCID 9899188, compound

Participants

Reaction Steps

4.72 g (20 mmol) XIX were heated under reflux for 15 h in a mixture of 200 ml tetrahydrofuran, 100 ml water and 10 ml concentrated H2SO4. Ethyl acetate and saturated NaCl solution were added to the reaction solution. The phases were separated and the aqueous phase was extracted three times with ethyl acetate. The combined organic phases were dried over Na2SO4 and freed from the solvent. Flash chromatography (200 g SiO2, n-hexane:ethyl acetate=1:2+1% acetic acid, applied with ethanol) produced 2.78 g (13 mmol, 67%) XX.

Provenance & Evidence