Phosphorus oxychloride → HCID 57503298, compound

Participants

Reaction Steps

A mixture of 215 (20 mg) and POCl3 (2 ml) is heated at reflux for 3 hours. The excess of POCl3 is removed. Ethyl acetate (10 mL) is added, and the mixture is washed with saturated NaHCO3 (5 mL), brine (5 mL), and dried over MgSO4. After evaporation of the solvent, the residue is purified by PTLC with 5% MeOH in dichloromethane to give the title product (213). 1H NMR δ (CDCL3) 0.99 (t, 3H, J=7.5 Hz), 1.55 (p, 2H, J=7.2 Hz), 2.62 (s, 3H), 2.92 (t, 2H, J=7.5 Hz), 5.92 (s, 2H), 6.87 (dd, 1H, J=8.1, 3 Hz), 7.15 (s, 1H), 7.22 (s, 1H), 7.85 (q, 1H, J=8.1 Hz), 8.06 (s, 1H), 8.14 (d, 1H, J=8.1 Hz), 8.57 (s, 1H). LC-MS: (M+1) 351.12.

Provenance & Evidence