反应详情

温度

60 °C

3.96 g of methyl 2-(dimethoxymethyl)-3-hydroxyacrylate sodium salt was suspended in 40 ml of ethanol, and 3.13 g of cyclohexylhydrazine hydrochloride was added. The mixture was stirred at 60° C. for 4 hours and then cooled to room temperature. After 50 ml of water was added, the reaction mixture was concentrated to 50 ml under reduced pressure. The concentrated solution was extracted with ethyl acetate. The organic layer was washed with aqueous saturated sodium chloride, dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 3.01 g of methyl 1-cyclohexyl-1H-pyrazole-4-carboxylate.

1. temperaturecooled to room temperature
2. concentrationthe reaction mixture was concentrated to 50 ml under reduced pressure
3. extractionThe concentrated solution was extracted with ethyl acetate
4. washThe organic layer was washed with aqueous saturated sodium chloride
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated under reduced pressure