反应详情

A solution of 10.0 g (0.1 mol) of 3-methyl-2-butenoic acid in 200 ml of THF is mixed with 9.4 ml (0.1 mol) of ethyl chloroformate and 14.1 ml (0.1 mol) of triethylamine at 0° C. After 10 minutes at room temperature, 10.6 ml (0.11 mol) of 4-fluoroaniline is added to it. The batch is stirred for 1 hour at room temperature, diluted with water and extracted with ethyl acetate (1 l). The organic phase is washed with saturated NaCl, dried (Na2SO4) and concentrated by evaporation in a vacuum. The residue is purified by column chromatography on silica gel with hexane-ethyl acetate. Yield 18.8 g.

1. extractionextracted with ethyl acetate (1 l)
2. washThe organic phase is washed with saturated NaCl
3. dry with materialdried (Na2SO4)
4. concentrationconcentrated by evaporation in a vacuum
5. customThe residue is purified by column chromatography on silica gel with hexane-ethyl acetate