Hydrochloric Acid → HCID 54002400, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of 12.5 g of the product obtained in example 1, in 120 ml of acetic acid was added 40 ml of concentrated hydrochloric acid. The resulting mixture was heated at 60° C. for 1 h. At the end of this time, the solvent was removed under reduced pressure and the residue was diluted with acetone. The resulting white solid was filtered and washed with excess of acetone. The solid was suspended in methanol and the pH was adjusted to 7 by the addition of triethylamine. The solvent was removed under reduced pressure and the resulting residue was dissolved in ethyl acetate and washed with water followed by brine. The organic layer was dried over anhydrous sodium sulphate and the solvent was removed by distillation under reduced pressure. The crude product was purified by column chromatography on silicagel using 2 to 10% (gradient elution) of methanol in chloroform to afford 9.8 g of the title compound.

Provenance & Evidence