反应详情

To a solution of 60% sodium hydride (496 mg) in DMF (10 mL) was added a solution of 1H-pyrazol-3-amine (1.03 g) in DMF (5 mL) under ice-cooling, followed by stirring at room temperature for 30 minutes. A solution of [(3-bromopropoxy)methyl]benzene (2.93 g) in DMF (10 mL) was added thereto under ice-cooling, followed by stirring at room temperature overnight. Saturated brine and saturated aqueous sodium bicarbonate were added thereto, followed by extraction with chloroform. The organic layer was dried over anhydrous magnesium sulfate and concentrated. The obtained crude product was purified by silica gel column chromatography (hexane:ethyl acetate=1:1-1:3) to obtain 1-[3-(benzyloxy)propyl]-1H-pyrazol-3-amine (835 mg) as a pale yellow oily substance.

1. temperaturecooling
2. temperatureunder ice-cooling
3. stirringby stirring at room temperature overnight
4. extractionfollowed by extraction with chloroform
5. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
6. concentrationconcentrated
7. customThe obtained crude product
8. customwas purified by silica gel column chromatography (hexane:ethyl acetate=1:1-1:3)