反应详情

To a solution of 4-nitro-1,3-phenylene diacetate (1.0 g) in chloroform (25 mL) was added aluminium chloride (2.23 g) with ice-cooling under nitrogen atmosphere. The reaction mixture was warmed to room temperature and stirred for 3 h. Then to the reaction mixture was added water (100 mL) and extracted with methylene chloride (30 mL×2). The combined organic layer was washed with 1N hydrochloric acid (25 mL) and saturated brine (25 mL) successively, dried over anhydrous sodium sulfate and was concentrated under reduced pressure. The residue was purified by column chromatography over silica gel using hexane/ethyl acetate (20:1) to give the title compound (610 mg).

1. temperaturecooling under nitrogen atmosphere
2. extractionextracted with methylene chloride (30 mL×2)
3. washThe combined organic layer was washed with 1N hydrochloric acid (25 mL) and saturated brine (25 mL) successively
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationwas concentrated under reduced pressure
6. customThe residue was purified by column chromatography over silica gel