反应详情

5,6,6a,7,8,9-Hexahydro-4H-2-phenalenylamine (0.130 g) was dissolved in pyridine (5 ml) and anhydrous benzene (2 ml), the solution was added with 4-chlorosulfonylbenzoic acid (0.161 g) and 4-dimethylaminopyridine (one pellet), and the mixture was stirred overnight at room temperature. The reaction mixture was made to be at 60° C., stirred for 3 hours, left to cool, then added with 2 N aqueous hydrochloric acid and thereby made acidic, and the mixture was extracted with chloroform. The organic layer was washed with saturated brine, and dried over anhydrous sodium sulfate. The organic layer was concentrated under reduced pressure, and the resulting residue was recrystallized from ethyl acetate-n-hexane to obtain the title compound (0.194 g, yield: 75%) as brown needles (melting point: 266-268° C.).

1. customto be at 60° C.
2. stirringstirred for 3 hours
3. waitleft
4. temperatureto cool
5. extractionmade acidic, and the mixture was extracted with chloroform
6. washThe organic layer was washed with saturated brine
7. dry with materialdried over anhydrous sodium sulfate
8. concentrationThe organic layer was concentrated under reduced pressure
9. customthe resulting residue was recrystallized from ethyl acetate-n-hexane