反应详情

At 23°-25° C., a solution of 2-ethoxy-4-cyanomethyl-benzoate (2.35 g, 10 mmol) and α-cyclohexylmethyl-2-piperidino-benzyl alcohol (2.88 g, 10 mmol) in o-dichlorobenzene (15 ml) is added dropwise to a mixture of concentrated sulphuric acid (15 ml) and o-dichlorobenzene (15 ml). The mixture is stirred for 2 hours at ambient temperature. The o-dichlorobenzene phase is then separated off and the residue is added to ice. After being made alkaline with soda solution, it is extracted with chloroform. The extracts are dried over sodium sulphate and concentrated by evaporation. The residue is purified by column chromatography on silica gel (toluene/acetone=10/1).

1. customThe o-dichlorobenzene phase is then separated off
2. additionthe residue is added to ice
3. extractionis extracted with chloroform
4. dry with materialThe extracts are dried over sodium sulphate
5. concentrationconcentrated by evaporation
6. customThe residue is purified by column chromatography on silica gel (toluene/acetone=10/1)