Chloroform → HCID 57625947, compound

Participants

Reaction Steps

To a 50 mL flask was added 3 (2.04 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 1.67 g (82%) of 4 as a yellow solid: TLC Rf 0.41 (Hexane/EtOAc 15:1); mp 42.4-43.8° C.; 1H NMR (DMSO-d6) δ 1.79 (q, 2H, J=8 Hz), 1.87 (q, 2H, J=8 Hz), 2.63 (s, 3H), 2.75 (d, 4H, J=8 Hz).

Provenance & Evidence