反应详情

To bis(2,2,2-trichloroethyl) 4-bromo-1-methyl-1H-pyrazol-3-ylimidodicarbonate (5.73 g, 10.87 mmol) in THF (50 mL) was added dropwise an aqueous potassium hydroxide solution (2.0 M, 5.7 mL, 11.4 mmol) and the reaction was stirred at rt for 30 minutes. An additional aliquot of aqueous potassium hydroxide (2.0 M, 1.4 mL, 2.8 mmol) was added and the reaction stirred for ½ hour. The reaction was quenched with aqueous saturated ammonium chloride, water was added, the product extracted with Et2O (2×), dried over Na2SO4, concentrated in vacuo and purified by flash chromatography over silica gel (EtOAc/Hex, 1/1) to afford 2,2,2-trichloroethyl 4-bromo-1-methyl-1H-pyrazol-3-ylcarbamate.

1. stirringthe reaction stirred for ½ hour
2. customThe reaction was quenched with aqueous saturated ammonium chloride, water
3. additionwas added
4. extractionthe product extracted with Et2O (2×)
5. dry with materialdried over Na2SO4
6. concentrationconcentrated in vacuo
7. custompurified by flash chromatography over silica gel (EtOAc/Hex, 1/1)