Hydrochloric Acid → HCID 58071508, compound

Participants

Reaction Conditions

Reaction Steps

Diethenyl(3-methoxy-4-nitrophenyl)phosphane oxide (INTERMEDIATE 58) (0.45 g, 1.78 mmol) and diethyl malonate (0.285 g, 1.78 mmol) were added to a 15 mL round-bottomed flask. DMSO (10 mL) was added to give a brown solution. Potassium carbonate (0.368 g, 2.67 mmol) was added. The reaction was heated to 75° C. and stirred at that temp for 1 h. The reaction was cooled to RT, and the solution was poured into an HCl solution (1N, 40 mL). The mixture was extracted with EtOAc (3×10 mL), and the combined organic layers were dried (Na2SO4) and concentrated to give the crude product. The crude product was added to a silica gel column (40 g) and eluted with MeOH/DCM (0-5%). The collected fractions were concentrated to give the product (0.3 g, 41%).

Provenance & Evidence