反应详情

A solution of 5,6,6a,7,8,9-hexahydro-4H-2-phenalenylamine (0.260 g) in anhydrous benzene (10 ml) and pyridine (3 ml) was added with monomethyl terephthalate chloride (0.304 g), and the mixture was stirred at room temperature for 3 hours. The reaction mixture was added with 2 N aqueous hydrochloric acid and thereby made acidic, and the mixture was extracted with ethyl acetate. The organic layer was washed successively with water, 10% aqueous sodium carbonate, water and saturated brine, and then dried over anhydrous sodium sulfate. The organic layer was concentrated under reduced pressure, and the resulting residue was recrystallized from chloroform-n-hexane to obtain the title compound (0.460 g, yield: 95%) as colorless needles (melting point: 217-218° C.).

1. extractionmade acidic, and the mixture was extracted with ethyl acetate
2. washThe organic layer was washed successively with water, 10% aqueous sodium carbonate, water and saturated brine
3. dry with materialdried over anhydrous sodium sulfate
4. concentrationThe organic layer was concentrated under reduced pressure
5. customthe resulting residue was recrystallized from chloroform-n-hexane