反应详情

A solution of 0.9 g of 1-[6-(2,2-dichlorocyclopropylmethoxy)-5-fluoro-1-methyl-1H-indazol-3-yl]-ethanone oxime in 10 ml of N,N-dimethylformamide is added dropwise to a suspension of 0.2 g of sodium hydride in 15 ml of N,N-dimethylformamide and the reaction mixture is stirred at room temperature for 15 minutes. Then 1.04 g of 2-(α-bromo-o-tolyl)-3-methoxyacrylic acid methyl ester in 10 ml of N,N-dimethylformamide are added dropwise and the reaction mixture is stirred at room temperature for a further 3 hours. The mixture is then acidified with acetic acid and concentrated by evaporation in vacuo at approx. 50° C. The residue is dissolved in ethyl acetate and the solution is washed twice with water and once with saturated sodium chloride solution, dried with sodium sulfate and concentrated by evaporation in vacuo. Purification by flash chromatography (silica gel, ethyl acetate/hexane 1:1) yields the title compound having a melting point of 138-140° C.

1. stirringthe reaction mixture is stirred at room temperature for a further 3 hours
2. concentrationconcentrated by evaporation in vacuo at approx. 50° C
3. dissolutionThe residue is dissolved in ethyl acetate
4. washthe solution is washed twice with water and once with saturated sodium chloride solution
5. dry with materialdried with sodium sulfate
6. concentrationconcentrated by evaporation in vacuo
7. customPurification by flash chromatography (silica gel, ethyl acetate/hexane 1:1)