反应详情

A solution of 2-(2-amino-4-pyridyl)-2-bromo-1-(3-methylphenyl)ethanone hydrobromide (5.00 g, 12.3 mmol) and 2-chlorothiobenzamide (1.06 g, 11.9 mmol) in N,N-dimethylformamide (40 mL) was stirred for 14 hours at room temperature. Aqueous sodium hydrogen carbonate solution was poured into the reaction mixture, and extracted with ethyl acetate. The extracts were washed with water, dried, and concentrated. The residue was purified by silica gel column chromatography (hexaneethyl acetate=4:1 to 2:1) to obtain a crystal. This crystal was washed with isopropyl ether, to obtain a title compound (3.15 g, yield 81%).

1. extractionextracted with ethyl acetate
2. washThe extracts were washed with water
3. customdried
4. concentrationconcentrated
5. customThe residue was purified by silica gel column chromatography (hexaneethyl acetate=4:1 to 2:1)
6. customto obtain a crystal
7. washThis crystal was washed with isopropyl ether