Methyl acetoacetate → HCID 24810447, compound

Participants

Reaction Steps

2 mmol 2,4,6-Trifluorobenzamidine acetate (Judkins, B. D., Allen, D. G., Cook, T. A. Synth. Commun. 1996, 26(23):4351-4367), 2 mmol 2-chloro-4-fluorobenzaldehyde, 2 mmol methyl acetoacetate and 2.2 mmol sodium acetate were reacted under reflux in 10 ml anhydrous ethanol for 20 hr, concentrated, and then ethyl acetate and water were added to separate the layers. The ethyl acetate layer was dried over anhydrous sodium sulfate, and separated by a column chromatography to obtain 0.29 g of a colorless fine needle crystal with mp 184-186° C.; 1H-NMR (400 MHz, DMSO-d6) δ 1.02-1.05 (3H, t, J=7.3 Hz); 2.32 (3H, s); 3.92-3.95 (2H, m, J=7.3 Hz); 5.97 (1H, s); 7.21-7.45 (5H, m); MS (EI) 426 (M+).

Provenance & Evidence