反应详情

温度

130 °C

A mixture of 2-chloro-5-(4-methoxyphenyl)pyridine (200 mg, 0.91 mmol), dry DMSO (2.0 mL) and 1-isopropylpiperazine (500 mg, 3.9 mmol) was stirred and heated on a 130° C. oil-bath overnight, then at 150° C. for 4 h, left 2 days at rt and finally heated at 140° C. overnight. The reaction mixture was allowed to cool and then poured into water (100 mL). The mixture was extracted with ethyl acetate (100 mL), and the organic extract was washed with water and dried (MgSO4). The solvent was evaporated to give a solid residue which was dissolved into 0.5 N hydrochloric acid (20 mL). A small insoluble solid was removed by filtration, and the aqueous solution was evaporated to give a residue which was re-evaporated with absolute ethanol. The resulting solid was re-crystallised from absolute ethanol to give 210 mg (60%) of 1-[5-(4-methoxyphenyl)pyridin-2-yl]-4-isopropylpiperazine, dihydrochloride.

1. waitleft 2 days at rt
2. temperaturefinally heated at 140° C. overnight
3. temperatureto cool
4. extractionThe mixture was extracted with ethyl acetate (100 mL)
5. extractionthe organic extract
6. washwas washed with water
7. dry with materialdried (MgSO4)
8. customThe solvent was evaporated
9. customto give a solid residue which
10. customA small insoluble solid was removed by filtration
11. customthe aqueous solution was evaporated
12. customto give a residue which
13. customwas re-evaporated with absolute ethanol
14. customThe resulting solid was re-crystallised from absolute ethanol