Formic Acid → HCID 12992513, compound

Participants

Reaction Steps

Formic acid (0.18 mL, 4.57 mmol) was added dropwise to a flask containing acetic anhydride (0.36 mL, 3.84 mmol) at 0° C. The mixture was then heated for 2 hrs. at 50° C. At this time the mixture was cooled to room temperature and 0.29 mL of THF was added. In a separate flask the product from Step 1, Example 13 (150 mg, 3.17 mmol) was suspended in 1.2 mL of THF and cooled to −20° C. To this suspension was added the acetic formic anhydride solution (0.088 mL). The reaction was stirred for 2 hrs. then was concentrated to dryness and pumped dry under high vacuum. The crude product was chromatographed in silica gel using 7% MeOH:0.5% NH4OH:methylene chloride as the eluant to obtain 65 mg of the title compound.

Provenance & Evidence