反应详情

To a suspension of electrolytic iron powders (9 g) in 5% acetic acid (200 g) under reflux, a solution of N-(2-fluoro-5-nitrophenyl)-3,4,5,6-tetrahydrophthalimide (VII) (15 g) in acetic acid (50 g) was added dropwise. After completion of the addition, the resultant mixture was heated under reflux for 30 minutes, cooled and filtered. The filtrate was diluted with water and extracted with ethyl acetate. The extract was concentrated, and the precipitated crystals were collected by filtration to give 10.5 g of N-(2-fluoro-5-aminophenyl)-3,4,5,6-tetrahydrophthalimide (VIII). M.P., 117°-119° C.

1. temperatureunder reflux
2. additionAfter completion of the addition
3. temperatureunder reflux for 30 minutes
4. temperaturecooled
5. filtrationfiltered
6. additionThe filtrate was diluted with water
7. extractionextracted with ethyl acetate
8. concentrationThe extract was concentrated
9. filtrationthe precipitated crystals were collected by filtration