反应详情

4-Fluoro-5-(5-isoquinolylsulfanyl)-2-nitroaniline 1.60 g (5.1 mmol) was dissolved in concentrated hydrochloric acid 30 ml, stannous chloride dihydrate 4.10 g (18.2 mmol) was added, and the mixture was stirred for 2 hours at room temperature. After 50% sodium hydroxide was added, the resulting alkaline solution was extracted with ethyl acetate. The organic layer was washed with water and saturated sodium chloride, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The resulting residue was recrystallized from ethyl acetate-n-hexane to obtain 4-fluoro-5-(5-isoquinolylsulfanyl)-1,2-benzenediamine 1.00 g (69.1%).

1. extractionthe resulting alkaline solution was extracted with ethyl acetate
2. washThe organic layer was washed with water and saturated sodium chloride
3. dry with materialdried over anhydrous sodium sulfate
4. concentrationconcentrated under reduced pressure
5. customThe resulting residue was recrystallized from ethyl acetate-n-hexane