Water → 4-Iodo-1-(propan-2-yl)-1H-pyrazole

Temperature

0 °C

Under argon atmosphere, 96 mg of 60% sodium hydride was suspended in 6 ml of N,N-dimethylformamide, and 388 mg of 4-iodo-1H-pyrazol was added at 0° C., and the mixture was stirred at 0° C. for 30 minutes. Subsequently, 0.21 ml of 2-bromopropane was added and the reaction mixture was stirred at 100° C. for 2 hours. The reaction solution was added with water. The solution was subjected to extraction with ethyl acetate. The organic layer was washed with brine and then dried over magnesium sulfate. The solvent was distilled off under reduced pressure, and then the obtained residue was purified by silica gel column chromatography to obtain 328 mg of the objective compound.

1. stirringthe reaction mixture was stirred at 100° C. for 2 hours
2. extractionThe solution was subjected to extraction with ethyl acetate
3. washThe organic layer was washed with brine
4. dry with materialdried over magnesium sulfate
5. distillationThe solvent was distilled off under reduced pressure
6. customthe obtained residue was purified by silica gel column chromatography

ORD record

ord-e20fe6eb0c47442d9cd38386c68181a6

Source dataset

uspto-grants-2013_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08586591B2