反应详情

温度

70 °C

The resulting 1-(3,3-diphenylpropyl )homopiperazine was dissolved in 3 mL of acetonitrile followed by adding 213 mg of 4-nitrobenzyl bromide and 144 mg of potassium carbonate. The mixture was stirred at 70° C. for 14 hours and allowed to cool to room temperature and the solvent was removed under reduced pressure. 20 mL of aqueous 2N sodium hydroxide was added and the mixture was extracted with 20 mL×2 of ethyl acetate. The organic layers were combined, washed with 20 mL of saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate, filtered, concentrated, and purified by column chromatography (silica gel, ethyl acetate) to obtain 255 mg of the titled compound. This was treated with a hydrogen chloride solution in ether and the solvent was removed under reduced pressure; and the residue was dried to obtain the hydrochloride salt of the titled compound.

1. temperatureto cool to room temperature
2. customthe solvent was removed under reduced pressure
3. addition20 mL of aqueous 2N sodium hydroxide was added
4. extractionthe mixture was extracted with 20 mL×2 of ethyl acetate
5. washwashed with 20 mL of saturated aqueous sodium chloride
6. dry with materialdried over anhydrous magnesium sulfate
7. filtrationfiltered
8. concentrationconcentrated
9. custompurified by column chromatography (silica gel, ethyl acetate)