反应详情

2 mmol 2,6-Difluorobenzamidine hydrochloride (Boere, R. J., Oakley, R. T., Read, R. V., J. Organometal. Chem. 1987, 331:161-167), 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 0.21 g of a colorless fine needle crystal with mp 126-128° C.; 1H-NMR (400 MHz, DMSO-d6) δ 2.87 (3H, s); 3.45 (3H, s); 5.92 (1H, s); 7.10-7.38 (6H, m); 9.87 (1H, s); MS (EI) 394.0 (M+).

1. concentrationconcentrated
2. additionethyl acetate and water were added
3. customto separate the layers
4. dry with materialThe ethyl acetate layer was dried over anhydrous sodium sulfate
5. customseparated by a column chromatography