Phosphorus oxychloride → HCID 24958350, compound

Participants

Reaction Steps

The product of example 4 (200 mg, 0.46 mmol) was heated in freshly distilled P(O)Cl3 (10 ml) to 90° C. for 3 hours and then solvents were removed under vacuum. The residue was dissolved in CH2Cl2 and washed with aqueous NaHCO3 and evaporated. The residue was purified by silica gel column chromatography using increasing gradient of CH2Cl2 in hexane to pure CH2Cl2. Yield (40%); 1H NMR (300 MHz, CDCl3) δ: 3.77 (s, 6H, 2×OMe), 3.79 (s, 3H, OMe), 3.94 (s, 3H, OMe), 6.49 (d, J=3.0 Hz, 1H), 6.71 (s, 2H), 7.08 (d, J=3.0 Hz, 1H), 7.27 (d, J=9.0 Hz, 1H), 7.53 (dd, J=9.0, 1.2 Hz, 1H), 8.05 (d, J=1.2 Hz, 1H), 8.72 (bs, 1H).

Provenance & Evidence