反应详情

In 150 ml of absolute ethanol was dissolved 2.26 g of 4-acetyl-1-(2-pyridyl)-5-methylpyrazole, and 2.94 g of 1-(3,5-dichlorophenyl)piperazine hydrochloride and 0.9 g of p-formaldehyde were added to the solution, followed by refluxing for 6 hours. To the reaction mixture was further added 0.40 g of p-formaldehyde, and the refluxing was continued for an additional 24 hour period. About a half of the ethanol was removed by evaporation, and the precipitate was collected by filtration. The precipitate was dissolved in chloroform, washed successively with a saturated aqueous solution of sodium hydrogencarbonate and a saturated aqueous solution of sodium chloride, and dried over anhydrous sodium sulfate. The solvent was removed by evaporation, and the residue was subjected to column chromatography on silica gel using a mixture of chloroform-methanol (50:1 by volume) as a developing solvent. The fraction containing the desired compound was concentrated. A 1N hydrochloric acid/ethanol solution was added to the residue, followed by concentration. The residue was recrystallized from ethanol to yield 2.90 g of the title compound.

1. additionwere added to the solution
2. temperatureby refluxing for 6 hours
3. customAbout a half of the ethanol was removed by evaporation
4. filtrationthe precipitate was collected by filtration
5. dissolutionThe precipitate was dissolved in chloroform
6. washwashed successively with a saturated aqueous solution of sodium hydrogencarbonate
7. dry with materiala saturated aqueous solution of sodium chloride, and dried over anhydrous sodium sulfate
8. customThe solvent was removed by evaporation
9. additiona mixture of chloroform-methanol (50:1 by volume) as a developing solvent
10. additionThe fraction containing the desired compound
11. concentrationwas concentrated
12. additionA 1N hydrochloric acid/ethanol solution was added to the residue
13. concentrationfollowed by concentration
14. customThe residue was recrystallized from ethanol