反应详情

3 g (11.9 mmols) of 3-ethoxy-4-ethoxycarbonylphenylacetic acid, 3.7 g (14.3 mmols) of triphenylphosphine, 3.3 ml (23.8 mmols) of triethylamine and 1.15 ml (11.9 mmols) of carbon tetrachloride were added successively to a solution of 2.9 g (11.9 mmols) of 3-methyl-1-(2-piperidino-phenyl)-1-butylamine in 29 of acetonitrile. The mixture was then stirred for 15 hours at room temperature, the solvent was removed in vacuo, and the residue was taken up in a mixture of ethyl acetate and water. The organic phase was dried over sodium sulfate, filtered and concentrated by evaporation in vacuo. The evaporation residue was purified by column chromatography on silaca gel (toluene/acetone=10/1).

1. customthe solvent was removed in vacuo
2. additionthe residue was taken up in a mixture of ethyl acetate and water
3. dry with materialThe organic phase was dried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated by evaporation in vacuo
6. customThe evaporation residue was purified by column chromatography on silaca gel (toluene/acetone=10/1)