反应详情

温度

60 °C

N-(3-Cyano-4-neopentyloxyphenyl)-5-methylpyrazole-4-carboxamide (2.4 g), potassium carbonate (1.1 g), potassium iodide (1.4 g) and ethyl bromoacetate (1.4 g) were added to a mixed solvent of dimethylformamide (24 ml) and toluene (24 ml) and the mixture was stirred at 60° C. for 4 h. The reaction mixture was added into water, washed with dilute hydrochloric acid and saturated brine, and dried over anhydrous magnesium sulfate, after which the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (mobile phase: chloroform). Methylene chloride was added to the obtained oily substance to allow crystallization. The crystals were recrystallized from a mixed solvent of methylene chloride-n-hexane to give the title compound (0.7 g), melting point: 240° C.

1. washwashed with dilute hydrochloric acid and saturated brine
2. dry with materialdried over anhydrous magnesium sulfate
3. customafter which the solvent was evaporated under reduced pressure
4. customThe residue was purified by silica gel column chromatography (mobile phase: chloroform)
5. additionMethylene chloride was added to the obtained oily substance
6. customcrystallization
7. customThe crystals were recrystallized from a mixed solvent of methylene chloride-n-hexane