反应详情

0.21 Gram of 4-(3-chlorophenyl)-1-(2,3-epoxypropyl)piperazine was added to a solution containing 0.21 g of 1-amino-2,3-dihydro-7-hyroxy-2,2,4,6-tetramethyl-1H-indene hydrochloride in 10 ml of ethanol solution, and the mixture was refluxed for 5 hours. After the reaction was completed, the reaction mixture was concentrated by removing the solvent under a reduced pressure, the residue thus obtained was alkalified with 10%-sodium bicarbonate aqueous solution, then extracted with 100 ml of methylene chloride. The extract was washed there times with 100 ml of water each time, then dried with anhydrous magnesium sulfate. The methylene chloride extract was concentrated by removing the solvent under a reduced pressure, and the residue was purified by a silica gel column chromatography (eluent: ethyl acetate: n-hexane=1:1) to obtain 0.21 g of 1-{3-[4-(3-chlorophenyl)-1-piperazinyl]-2-hydroxypropylamino}-2,3-dihydro-7-hydroxy-2,2,4,6-tetramethyl-1H-indene.

1. temperaturethe mixture was refluxed for 5 hours
2. concentrationthe reaction mixture was concentrated
3. customby removing the solvent under a reduced pressure
4. customthe residue thus obtained
5. extractionextracted with 100 ml of methylene chloride
6. washThe extract was washed there times with 100 ml of water each time
7. dry with materialdried with anhydrous magnesium sulfate
8. extractionThe methylene chloride extract
9. concentrationwas concentrated
10. customby removing the solvent under a reduced pressure
11. customthe residue was purified by a silica gel column chromatography (eluent: ethyl acetate: n-hexane=1:1)