反应详情

A mixture of 4-fluoronitrobenzene (30.34 g, 0.22 mole), cis-2,5-dimethylpiperazine (25 g, 0.22 mole) and sodium bicarbonate (24 g, 0.28 mole) in n-pentanol (150 ml) was heated under nitrogen at 90°-100° for 18 hours. After filtration, the n-pentanol was removed under reduced pressure and the residue was partitioned between methylene chloride and water. The organic phase was separated, washed again with water, dried over magnesium sulphate, and concentrated under reduced pressure. The residue was triturated with ice water to yield a yellow solid. The solid was filtered off and dried to yield the title compound, m.p. 93°-4° (37 g, 71%).

1. temperaturewas heated under nitrogen at 90°-100° for 18 hours
2. filtrationAfter filtration
3. customthe n-pentanol was removed under reduced pressure
4. customthe residue was partitioned between methylene chloride and water
5. customThe organic phase was separated
6. washwashed again with water
7. dry with materialdried over magnesium sulphate
8. concentrationconcentrated under reduced pressure
9. customThe residue was triturated with ice water
10. customto yield a yellow solid
11. filtrationThe solid was filtered off
12. customdried