反应详情

温度

140 °C

A mixture of 2-(2-chloro-4-methoxy-phenyl)-3-(2-methyl-pyridin-4-yl)-3-oxo-propionic acid methyl ester (13.95 g), sodium chloride (2.71 g), water (1.14 mL) and DMSO (400 mL) was heated to 140° C. for 3 hours. Stirring was continued overnight at r.t. The reaction mixture was poured into ice/water and extracted two times with ethyl acetate. The organic layers were washed with brine, dried over Na2SO4, filtered and the solvent was evaporated. The residue was purified by flash chromatography (silica gel, gradient of heptane in ethyl acetate) to give the title compound as a yellow solid (7.56 g, 62%). MS (m/e)=276.2 [MH+].

1. extractionextracted two times with ethyl acetate
2. washThe organic layers were washed with brine
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. customthe solvent was evaporated
6. customThe residue was purified by flash chromatography (silica gel, gradient of heptane in ethyl acetate)