HCID 86725347, compound → HCID 90272315, compound

Participants

Reaction Conditions

Reaction Steps

Poly phosphoric acid (˜1 ml) was added to a vial containing the product from step (b) (0.255 g, 0.50 mmol) and heated to 90° C. for 20 minutes. Water was added to the reaction mixture and extracted with dichloromethane (3×). The organic layers were washed with saturated sodium bicarbonate, and brine. To the crude material was added 8 ml of methanol, 5 ml of water, and potassium carbonate (˜100 mg). The reaction mixture was allowed to stir at room temperature for 16 hours. The reaction mixture was concentrated and to this was added 2N HCl, and extracted with dichloromethane (3×). Purification by silica-gel chromatography (gradient elution: 0-20% methanol in dichloromethane) gave the sub-title compound as an off white solid (0.034 mg). MS: ESI (positive): 390 (M+H).

Provenance & Evidence