Ethyl Acetoacetate → HCID 24810555, compound

Participants

Reaction Steps

2 mmol 2-chlorothiazol-5-formamidine hydrochloride, 2 mmol 2-chloro-4-fluorobenzaldehyde, 2 mmol ethyl 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 yellow crystal with mp 159-162° C.; 1H-NMR (400 MHz, DMSO-d6) δ 1.0-1.03 (3H, m); 2.43 (3H, s); 3.92-3.95 (2H, m); 5.91 (1H, s); 7.16-7.41 (3H, m); 8.31 (1H, s); 9.69 (1H, s); MS (EI) 413.0 (M+).

Provenance & Evidence