反应详情

Sodium hydride (156 mg) was added to a solution of 3-nitro-1H-pyrazole (196 mg) in anhydrous DMF (2 mL) under cooling with ice, and the mixture was stirred at room temperature for 15 minutes. A solution of 1-chloro-N,N,2-trimethylpropan-2-amine in DMF (0.52 mL) was added to the resultant mixture, and the mixture was stirred at room temperature for about 24 hours. A saturated aqueous ammonium chloride solution (25 mL) and ethyl acetate (25 mL) were added to the reaction mixture and stirred under cooling with ice. The organic layer was separated, washed with saturated brine (100 mL), dried over anhydrous sodium sulfate, and filtrated, and the filtrate was concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (neutral spherical silica gel, ethyl acetate:hexane=1:1) to give N,N,2-trimethyl-1-(3-nitro-1H-pyrazol-1-yl)propan-2-amine as yellow powder crystals (90.9 mg, yield: 25%).

1. temperatureunder cooling with ice
2. stirringthe mixture was stirred at room temperature for about 24 hours
3. stirringstirred
4. temperatureunder cooling with ice
5. customThe organic layer was separated
6. washwashed with saturated brine (100 mL)
7. dry with materialdried over anhydrous sodium sulfate
8. filtrationfiltrated
9. concentrationthe filtrate was concentrated under reduced pressure
10. customThe obtained residue was purified by silica gel column chromatography (neutral spherical silica gel, ethyl acetate:hexane=1:1)