HCID 59603146, compound → HCID 59603182, compound

Participants

Reaction Steps

A stirred solution of 3 (1.2 g, 4.0 mmol) in acetic acid (35 mL) was refluxed for 16 h. After cooling, the solution was evaporated to dryness. The crude product was adsorbed on silica gel and purified by flash chromatography, eluting with hexane/EtOAc (2:1) to give 4 (230 mg, 28%) as a white solid. 1H NMR (500 MHz, CDCl3): δ: 9.89 (1H, s, CHO), 7.50 (1H, s, H-3), 6.69 (1H, d, J4,6=2.2 Hz, H-6), 6.64 (1H, d, J4,6=2.2 Hz, H-4), 4.01 (3H, s, OMe), 3.87 (3H, s, OMe). 13C NMR CDEPT 135, (500 MHz, CDCl3): δ: 179.91 (CHO), 153.37 (C-2), 116.10 (C-3), 101.80 (C-6), 94.90 (C-4), 56.20 (OMe), 55.88 (OMe).

Provenance & Evidence