反应详情

温度

160 °C

A mixture of 0.43 g of 1-[N-(2-nitrophenyl)-2-aminoethyl]-4-(2-methoxyphenyl)piperazine (prepared as described in U.S. Pat. No. 3,472,854), 0.19 g of 2-bromopyridine, 0.17 g of anhydrous potassium carbonate and 0.01 g of powdered copper was heated to 100° C., and maintained at that temperature for 3 h, followed by the addition of another 0.138 g of 2-bromopyridine, and the heating of the mixture to 160° C. for 24 h. After cooling the mixture to room temperature and extraction with ethyl acetate (2×20 mL), the combined organic phases were then washed with water, dried on sodium sulphate, and evaporated to dryness in vacuo. The obtained crude was next purified by flash chromatography (ethyl acetate-petroleum ether 7:3). The recovered fractions, after evaporation to dryness, afforded 0.25 g of the compound of Example 11 (52%).

1. customprepared
2. temperaturemaintained at that temperature for 3 h
3. temperatureAfter cooling the mixture to room temperature
4. extractionextraction with ethyl acetate (2×20 mL)
5. washthe combined organic phases were then washed with water
6. customdried on sodium sulphate
7. customevaporated to dryness in vacuo
8. customThe obtained crude
9. customwas next purified by flash chromatography (ethyl acetate-petroleum ether 7:3)
10. customThe recovered fractions, after evaporation to dryness