反应详情

To 4-(2-fluoro-4-nitrophenoxy)-2-[(pyrrolidin-1-yl)carbonylamino]pyridine (2.927 g) dissolved in ethanol (100 ml)-water (20 ml) were added electrolytic iron powder (3.0 g) and ammonium chloride (6.0 g), followed by heating under reflux for 1 hr. The reaction mixture was cooled down to room temperature, and then ethyl acetate-tetrahydrofuran (1:1) was added thereto, followed by stirring. An insoluble portion was filtered through celite, and washed with ethyl acetate and water. The organic layer of the filtrate was separated, washed with water and brine in this order, and dried over anhydrous sodium sulfate. The solvent was evaporated under a reduced pressure to give a residue, to which ethyl acetate-hexane was added to suspend. Crystals was filtered off and dried under aeration to provide the titled compound (2.378 g, 89%) as pale brown crystals.

1. temperatureby heating
2. temperatureunder reflux for 1 hr
3. filtrationAn insoluble portion was filtered through celite
4. washwashed with ethyl acetate and water
5. customThe organic layer of the filtrate was separated
6. washwashed with water and brine in this order
7. dry with materialdried over anhydrous sodium sulfate
8. customThe solvent was evaporated under a reduced pressure
9. customto give a residue
10. filtrationCrystals was filtered off
11. customdried under aeration