Calciumoxide → HCID 18516277, compound

Participants

Reaction Steps

A suspension of Example 154 (0.15 g, 0.43 mmol) and calcium oxide (0.12 g, 2.15 mmol) in phenyl ether (10 mL) was heated to 220-250° C. The reaction was stirred 45 minutes over which reaction volume decreased due to evaporation of solvent. The reaction was cooled to room temperature and diluted with 10% MeOH/dichloromethane (25 mnL) then filtered. The filtrate was concentrated and residue was purified by preparative HPLC using a gradient of 30%-90% acetonitrile/water +0.1% TFA over 40 minutes. The product containing fractions were combined and neutralized with sat NaHCO3. The product crystalized upon standing for 3 days and was collected by filtration, and dried in a desiccator to yield the title compound as a tan needles (23 mg, 16%).

Provenance & Evidence