Sulfuric Acid → HCID 67099309, compound

Participants

Reaction Steps

In a 100 mL round bottom flask, 5 mL concentrated H2SO4 stirred at 0° C. was carefully treated with 2.5 g P2O5. The resulting mixture was stirred for 10 minutes. A mixture of diethyl 2-(4-(3-bromo-4-methoxyphenyl)-tetrahydro-2H-pyran-4-carbonyl)malonate (1.25 g, 2.7 mmol) in 2 mL EtOAc was added to the above H2SO4 mixture, and the mixture was stirred at room temperature for 2 hours, M+1=411/413. The reaction mixture was then poured into 200 g crushed ice. The mixture was extracted with EtOAc (3×50 mL). The combined organic layers were washed with brine (20 mL), dried over anhydrous Na2SO4, concentrated in vacuo, and purified by column chromatography eluting with 10-50% EtOAc/hexane to give 0.28 g of the product as a pale yellow solid. MS m/e=411/413 (M+H)+.

Provenance & Evidence