Chloroform → HCID 57428968, compound

Participants

Reaction Steps

To a 50 mL flask was added 4 (1.64 g, 10 mmol) and 10 mL POCl3. The resulting mixture was refluxed for 2 h, and the solvent was removed under reduced pressure to afford a dark residue. To this was added 30 mL of CHCl3 and 3 g of silica gel. The solvent was evaporated to afford a plug. Column chromatography of the plug with hexane:acetyl acetate=20:1 as eluent afford 1.55 g (85%) of 5 as a yellow solid: TLC Rf0.26 (Hexane/EtOAC 15:1); mp 47.6-48.1° C.; 1H NMR (DMSO-d6) δ 2.48 (s, 3 H) 2.63 (s, 3 H), 6.77 (s, 1 H).

Provenance & Evidence