Potassium Carbonate → HCID 22664926, compound

Participants

Reaction Steps

The intermediate 7-glycidylcoumarin was prepared in a reaction flask equipped with a reflux condenser containing 16.2 g 7-hydroxycournarin, 15.8 g epibromohydrin, 13.8 g potassium carbonate and 270 mL acetone. The reaction solution was boiled and refluxed overnight, cooled, treated with 100 mL 5% NaOH aqueous solution, and extracted three times with 80 mL methylene chloride. After evaporating the solvent, a crude yellow solid was obtained. The crude solid (1.5 g) was dissolved in a solution of 30 mL hexane and 20 mL acetone at 50° C. The hexane/acetone solution was then cooled at 0° C. for 2 to 3 hr. White crystals formed and were collected by filtering and dried to a white powder. Yield: 290 mg; melting point: 110-112° C.; Rf=0.6 (8% v/v ethyl acetate/CHCl3).

Provenance & Evidence