反应详情

A solution of crude 1-acetyl-4-[4-(6-bromohexyloxy)phenyl]piperazine (10.52 g) in methanol (105 ml) was treated with 28% sodium methoxide in methanol (105 ml), and the solution was refluxed for 7 hours. After cooling, the precipitate was removed by filtration. The filtrate was added to a mixture of methylene chloride and water. The organic layer was taken, dried over magnesium sulfate, filtered and evaporated to give a crude oil. This oil in methylene chloride (20 ml) was treated with acetic anhydride (6.4 ml) under ice-cooling. After 6 hours, the solution was added to a mixture of methylene chloride and water. The organic layer was taken, dried over magnesium sulfate, filtered and evaporated. The residue was purified by silica gel column chromatography eluting with a mixed solvent of methylene chloride-methanol (from 0% to 3% gradient elution) to give 1-acetyl-4-[4-(6-methoxyhexyloxy)phenyl]piperazine (5.38 g) as a pale red solid.

1. temperaturethe solution was refluxed for 7 hours
2. temperatureAfter cooling
3. customthe precipitate was removed by filtration
4. additionThe filtrate was added to a mixture of methylene chloride and water
5. dry with materialdried over magnesium sulfate
6. filtrationfiltered
7. customevaporated
8. customto give a crude oil
9. temperaturecooling
10. dry with materialdried over magnesium sulfate
11. filtrationfiltered
12. customevaporated
13. customThe residue was purified by silica gel column chromatography
14. washeluting with a mixed solvent of methylene chloride-methanol (from 0% to 3% gradient elution)