反应详情

N-(2-Fluoro-5-isopropoxyphenyl)-3,4,5,6-tetrahydrophthalimide (II: R=isopropyl) (2 g) and dicyclohexylamine (0.01 g) were dissolved in tetrachloroethylene (20 ml), and a solution of sulfuryl chloride (1 g) in tetrachloroethylene (5 ml) was added dropwise thereto at 80° C. in 2 hours. After completion of the addition, the resultant mixture was stirred at the same temperature as above for 2 hours, followed by extraction with ethyl acetate. The extract was concentrated, and the precipitated crystals were collected by filtration to give 1.85 g of N-(4-chloro-2-fluoro-5-isopropoxyphenyl)-3,4,5,6-tetrahydrophthalimide (I: R=isopropyl). M.P., 81°-82° C.

1. additionAfter completion of the addition
2. extractionfollowed by extraction with ethyl acetate
3. concentrationThe extract was concentrated
4. filtrationthe precipitated crystals were collected by filtration