Acetic Acid → HCID 86714685, compound

Participants

Reaction Conditions

Reaction Steps

Compound 7a (5 g, 0.011 mol) was added to methanol (25 mL) at 25-30° C. Acetic acid (15 mL) was added slowly to the reaction mixture over 30 min. The reaction mixture was stirred at 25-30° C. for 2 h. After 2 hrs, the reaction was monitored by TLC and showed completion. The reaction mixture was passed through a diatomaceous earth (Celite) pad and the pad was washed with methanol (25 mL). The filtrate was concentrated under reduced pressure at 50° C. The thus obtained residue was mixed with water (50 mL) and basified with aqueous NaHCO3 to pH 9.0. The aqueous layer was extracted with ethyl acetate (3×25 mL). The combined extract was washed with brine, dried over anhydrous Na2SO4, and concentrated under reduced pressure to provide the crude product (89%), which was used for next step without further purification.

Provenance & Evidence