反应详情

250 ml of toluene and 0.1 ml of aqueous 12.5 M sodium hydroxide solution were added to a mixture of 15.69 g of ethyl 3-amino-4-pyrazolecarboxylate, 24.34 g of (2-bromoethyl)benzene, 2.54 g of Adogen 464 and 27.74 g of potassium carbonate, and heated under reflux for 2.5 hours. The reaction solution was washed with 200 ml of water and dried over magnesium sulfate, and the solvent was distilled off under reduced pressure. The resulting residue was subjected to silica gel column chromatography (n-hexane--ethyl acetate=2:1→1:1→1:2) to obtain 16.94 g of 1-(2-phenylethyl)-3-amino-4-ethoxycarbonylpyrazole as colorless crystals.

1. temperatureheated
2. temperatureunder reflux for 2.5 hours
3. washThe reaction solution was washed with 200 ml of water
4. dry with materialdried over magnesium sulfate
5. distillationthe solvent was distilled off under reduced pressure