反应详情

温度

90 °C

To a solution of 1-(3-diethylaminopropyl)-3-[4-(2-methyl-4-nitrophenoxy)pyridin-2-yl]urea (794 mg) in ethanol (50 ml) were added electrolytic iron powder (442 mg), ammonium chloride (847 mg) and water (10 ml), followed by stirring at 90° C. for 1 hr. The reaction mixture was allowed to cool down to room temperature, insoluble matter was removed by filtration, and the filtrate was concentrated under reduced pressure. To the residue was added ethyl acetate (100 ml), washed with a saturated aqueous solution of sodium hydrogencarbonate, and dried over anhydrous sodium sulfate. The solvent was removed and the resultant residue was purified by silica gel column chromatography (Fuji Silysia NH, eluent; hexane:ethyl acetate=1:1 to 1:2, ethyl acetate, then ethyl acetate:methanol=20:1 to 10:1) to provide the titled compound (110 mg, 15%).

1. temperatureto cool down to room temperature
2. custominsoluble matter was removed by filtration
3. concentrationthe filtrate was concentrated under reduced pressure
4. additionTo the residue was added ethyl acetate (100 ml)
5. washwashed with a saturated aqueous solution of sodium hydrogencarbonate
6. dry with materialdried over anhydrous sodium sulfate
7. customThe solvent was removed
8. customthe resultant residue was purified by silica gel column chromatography (Fuji Silysia NH, eluent