Hydrochloric Acid → HCID 13746697, compound

Participants

Reaction Steps

The crude amide from Step A (4.34 g, 14.8 mmole) in pyridine (43.5 ml) was treated slowly under cooling (ice-bath) with trifluoroacetic anhydride (8.7 ml). The mixture was stirred for 1 hour at ambient temperature and then poured into a mixture of ice (400 g) and concentrated hydrochloric acid (50 ml). The product was extracted into ether and the ethereal extract was washed with water, then with 10% sodium carbonate solution and finally with saturated sodium chloride solution. After drying (MgSO4) the solution was evaporated to a tan colored solid (3.22 g). The product was purified by chromatography on Merck silica gel using toluene as solvent to give 2.45 g of the title compound. Melting point 142°-143° C. (from acetonitrile).

Provenance & Evidence