反应详情

温度

100 °C

A solution of 2-chloro-4-phenylpyridine (11.4 g) and 4-(4-methylbenzyl)piperazine (11.4 g) in 1,2,4-trichlorobenzene (40 cc) is heated for 5 hours at 170° C. After the mixture is cooled to a temperature in the region of 20° C., isopropyl ether (200 cc) is added. The precipitate formed is separated by filtration, washed with isopropyl ether (50 cc) and then dissolved in ethyl acetate (250 cc). 5N aqueous sodium hydroxide solution (16 cc) is added, followed by distilled water (100 cc). The organic solution is decanted and the aqueous phase washed with ethyl acetate (2×50 cc). The organic extracts are combined, dried over anhydrous magnesium sulphate, filtered and evaporated to dryness under reduced pressure (20 mm Hg; 2.7 kPa) at 40° C. The residue is dissolved in 2-propanol (75 cc); decolorizing charcoal (0.5 g) is added and the mixture is heated to 100° C. for 30 minutes, filtered on diatomaceous earth and cooled to 10° C. for 1 hour. The precipitate formed is separated by filtration and washed with 2-propanol (2×10 cc). 2-[4-(4-Methylbenzyl)-1-piperazinyl]-4-phenylpyridine (8 g), m.p. 103° C., is thereby obtained.

1. additionis added
2. customThe precipitate formed
3. customis separated by filtration
4. washwashed with isopropyl ether (50 cc)
5. dissolutiondissolved in ethyl acetate (250 cc)
6. addition5N aqueous sodium hydroxide solution (16 cc) is added
7. distillationby distilled water (100 cc)
8. customThe organic solution is decanted
9. washthe aqueous phase washed with ethyl acetate (2×50 cc)
10. dry with materialdried over anhydrous magnesium sulphate
11. filtrationfiltered
12. customevaporated to dryness under reduced pressure (20 mm Hg; 2.7 kPa) at 40° C
13. dissolutionThe residue is dissolved in 2-propanol (75 cc)
14. additiondecolorizing charcoal (0.5 g) is added
15. filtrationfiltered on diatomaceous earth
16. temperaturecooled to 10° C. for 1 hour
17. customThe precipitate formed
18. customis separated by filtration
19. washwashed with 2-propanol (2×10 cc)