反应详情

A mixture of 4-formyl-benzoic acid methyl ester (2.50 g), 1-(1-isocyano-ethanesulfonyl)-4-methyl-benzene (3.19 g), and potassium carbonate (2.76 g) in methanol (50 mL) is heated to reflux for 2 h. After cooling to room temperature, the mixture is poured onto water and extracted with dichloromethane. The organic phase is washed with water, dried over Na2SO4 and concentrated in vacuo. The residue is chromatographed on silica gel (dichloromethane/methanol 40:1) to afford the title compound. LC (method 6): tR=2.68 min; Mass spectrum (ESI+): m/z=218 [M+H]+.

1. temperatureis heated
2. temperatureto reflux for 2 h
3. additionthe mixture is poured onto water
4. extractionextracted with dichloromethane
5. washThe organic phase is washed with water
6. dry with materialdried over Na2SO4
7. concentrationconcentrated in vacuo
8. customThe residue is chromatographed on silica gel (dichloromethane/methanol 40:1)