反应详情

N-(2-Fluoro-5-isopropoxyphenyl)-3,4,5,6-tetrahydrophthalimide (II: R=isopropyl) (1 g) and dicyclohexylamine (0.01 g) were dissolved in tetrachloroethylene (20 ml), and chlorine (1 ml) was introduced therein at room temperature. The resultant solution was stirred at the room temperature for 2 hours. The reaction mixture was extracted with methylene chloride, and the extract was concentrated. The residue was purified by silica gel chromatography using a mixture of n-hexane and ethyl acetate as an eluent to give 0.9 g of N-(4-chloro-2-fluoro-5-isopropoxyphenyl)-3,4,5,6-tetrahydrophthalimide (I: R=isopropyl). M.P., 81°-82° C.

1. customat room temperature
2. extractionThe reaction mixture was extracted with methylene chloride
3. concentrationthe extract was concentrated
4. customThe residue was purified by silica gel chromatography
5. additiona mixture of n-hexane and ethyl acetate as an eluent