反应详情

温度

88 °C

A mixture of 2-nitrobenzaldehyde (10 g, 66 mmol), thiazole-2-carboximidamide hydrochloride (10.8 g, 66 mmol), ethyl 3-oxobutanoate (8.6 g, 66 mmol) and sodium acetate (5.5 g, 66 mmol) in ethanol (250 mL) was stirred at 88° C. for 16 hours, then cooled to 25° C. The resulting mixture was filtered and the filtrate was concentrated in vacuo. The residue was purified by a silica gel column chromatography (PETROLEUM ETHER/EtOAc (V/V)=3/1) to give the title compound as a light yellow solid (12 g, 48%). The compound was characterized by the following spectroscopic data:

1. temperaturecooled to 25° C
2. filtrationThe resulting mixture was filtered
3. concentrationthe filtrate was concentrated in vacuo
4. customThe residue was purified by a silica gel column chromatography (PETROLEUM ETHER/EtOAc (V/V)=3/1)