反应详情

20 ml of triethyl orthoformate and 0.1 g of toluenesulfonic acid were added to a solution of 3 g (8.8 mmol) of 2-chloro-5-(4-chloro-5-difluoromethoxy-1-methyl-1H-pyrazol-3-yl)-4-fluorobenzaldehyde in 50 ml of tetrahydrofuran. After the mixture had been refluxed for 2 hours, it was treated with 3 ml of triethylamine. The mixture was subsequently concentrated. The residue was treated with 50 ml of water. The product was subsequently extracted from the aqueous phase using ethyl acetate. The organic phase was then washed using saturated aqueous sodium hydrogen carbonate solution, dried over magnesium sulfate and finally concentrated. The crude product was purified by means of column chromatography on silica gel (eluent: hexane/ethyl acetate=9:1). Yield: 1 g.

1. temperatureAfter the mixture had been refluxed for 2 hours
2. concentrationThe mixture was subsequently concentrated
3. additionThe residue was treated with 50 ml of water
4. extractionThe product was subsequently extracted from the aqueous phase
5. washThe organic phase was then washed
6. dry with materialdried over magnesium sulfate
7. concentrationfinally concentrated
8. customThe crude product was purified by means of column chromatography on silica gel (eluent: hexane/ethyl acetate=9:1)