反应详情

温度

140 °C

A mixture of N-(1,3-benzoxazol-2-yl)benzene-1,4-diamine (0.50 g) and 2-chloro-3-nitropyridine (0.352 g) in NMP (3.0 ml) was stirred at 140° C. for 1.5 h. After this time, the reaction mixture was cooled to ambient temperature, diluted with water (50 ml), and extracted with ethyl acetate (3×100 ml). The combined organic extracts were washed with brine (100 mL), dried (Na2SO4), filtered and concentrated under reduced pressure. The residue obtained was purified by chromatography (silica, methylene chloride to 1:9 ethyl acetate/methylene chloride) to afford N-(1,3-benzoxazol-2-yl)-N′-(3-nitropyridin-2-yl)benzene-1,4-diamine (0.335 g) as a red solid.

1. temperatureAfter this time, the reaction mixture was cooled to ambient temperature
2. extractionextracted with ethyl acetate (3×100 ml)
3. washThe combined organic extracts were washed with brine (100 mL)
4. dry with materialdried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThe residue obtained
8. customwas purified by chromatography (silica, methylene chloride to 1:9 ethyl acetate/methylene chloride)