反应详情

温度

80 °C

To a stirred solution of 0.9 gram (0.002 mole) of N-(ethoxycarbonyl)-N′-[(2-chlorophenyl)(4-chlorophenyl)methyl]piperazine in 10 mL of tetrahydrofuran was added 10 mL of methanol and 10 mL of aqueous 50% sodium hydroxide. Upon completion of the addition the reaction mixture was warmed to 80° C., where it stirred for 24 hours. At the end of this time the reaction mixture was concentrated under reduced pressure. The concentrate was dissolved in chloroform, and the solution was stirred for 40 minutes. The resulting precipitate was collected by filtration. The filtrate was concentrated under reduced pressure, yielding 0.6 gram of crude material. The crude material was purified by preparative thin layer chromatography (TLC). Elution was accomplished with 1:1 acetone: methanol. The product-containing fractions were combined and concentrated under reduced pressure, yielding 0.4 gram of N′-[(2-chlorophenyl)(4-chlorophenyl)-methyl]piperazine. The NMR spectrum was consistent with the proposed structure.

1. additionUpon completion of the addition the reaction mixture
2. concentrationAt the end of this time the reaction mixture was concentrated under reduced pressure
3. dissolutionThe concentrate was dissolved in chloroform
4. stirringthe solution was stirred for 40 minutes
5. filtrationThe resulting precipitate was collected by filtration
6. concentrationThe filtrate was concentrated under reduced pressure
7. customyielding 0.6 gram of crude material
8. customThe crude material was purified by preparative thin layer chromatography (TLC)
9. washElution
10. concentrationconcentrated under reduced pressure