反应详情

4-Chloro-2-fluoro-5-isopropoxyaniline (1.3 g) and 3,4,5,6-tetrahydrophthalic anhydride (1.12 g) were dissolved in acetic acid (10 ml) and refluxed for 3 hours. The resultant mixture was allowed to cool to room temperature and poured into water, followed by extraction with ether. The ether extract was washed with water, dried over anhydrous sodium sulfate and subjected to filtration. The filtrate was concentrated under reduced pressure and the residue was purified by silica gel chromatography to obtain 1.0 g of N-(4-chloro-2-fluoro-5-isopropoxyphenyl)-3,4,5,6-tetrahydrophthalimide (Compound No. 1). M.P., 81°-82° C.

1. temperaturerefluxed for 3 hours
2. extractionfollowed by extraction with ether
3. extractionThe ether extract
4. washwas washed with water
5. dry with materialdried over anhydrous sodium sulfate
6. filtrationsubjected to filtration
7. concentrationThe filtrate was concentrated under reduced pressure
8. customthe residue was purified by silica gel chromatography