反应详情

温度

60 °C

To a mixture of 2,2,2-trichloroethyl[3-tert-butyl-1-(4-methylphenyl)-1H-pyrazol-5-yl]carbamate (101 mg) and (4-methyl-3-nitrophenyl)amine (38 mg) in DMSO (1 mL) was added iPr2NEt (44 under a nitrogen atmosphere and the mixture was stirred at 60° C. for 4 hr. The reaction mixture was diluted with EtOAc (2 mL) and successively washed with 1M HCl (2 mL×2), saturated aqueous NaHCO3 (2 mL) and brine (2 mL), dried over MgSO4 and filtered. The filtrate was evaporated in vacuo, and the residue was purified by silica gel column chromatography eluting with 2% MeOH in CH2Cl2 to give 1-[3-tert-butyl-1-(4-methylphenyl)-1H-pyrazol-5-yl]-3-(4-methyl-3-nitrophenyl)urea (96 mg).

1. washsuccessively washed with 1M HCl (2 mL×2), saturated aqueous NaHCO3 (2 mL) and brine (2 mL)
2. dry with materialdried over MgSO4
3. filtrationfiltered
4. customThe filtrate was evaporated in vacuo
5. customthe residue was purified by silica gel column chromatography
6. washeluting with 2% MeOH in CH2Cl2