反应详情

温度

140 °C

Concentrated HCl (17.6 mL) and pyridine (16 mL) were mixed together at room temperature. The resulting solution was heated on a sand bath while passing nitrogen over the surface of the solution and the distillate collected in a Dean-Stark trap. The internal temperature of the reaction was allowed to reach 215-220° C. over a 1 hour period. The solution was allowed to cool to 140° C. and 2-(2-methoxyphenyl)-1,10-phenanthroline hydrochloride chloride (6 g, 18.59 mMole) then added. With good stirring, the temperature of the resulting solution was allowed to rise back again to 215-220° C. and held at this temperature for 3 hours. The solution was then cooled to 100° C. and treated carefully with water (10 mL), then finally poured into an excess of water (70 mL) to precipitate a gummy solid. With good stirring, the pH of the solution was adjusted to 6-7 with solid Na2CO3. The orange solid was filtered off, washed well with water and dried. Yield of the 2-(2-hydroxyphenyl)-1,10-phenanthroline was 4.6 g.

1. temperatureThe resulting solution was heated on a sand bath
2. distillationthe distillate collected in a Dean-Stark trap
3. customto rise back again to 215-220° C.
4. waitheld at this temperature for 3 hours
5. temperatureThe solution was then cooled to 100° C.
6. customto precipitate a gummy solid
7. filtrationThe orange solid was filtered off
8. washwashed well with water
9. customdried