反应详情

To a solution of methyl 2-bromobenzoate (1.63 g, 17.8 mmol) in 1,6-dioxane (100 ml) at room temperature was added piperazine (15.3 g, 178 mmol) and K2CO3 (4.92 g, 35 mmol). The resulting mixture was heated to reflux for 7 days after which the reaction mixture was cooled to room temperature. The solvent and the excess piperazine were removed in vacuo along with heating with a hot water bath. The residue was dissolved in 1N NaOH solution, extracted with CH2Cl2 (6×30 ml), and dried over Na2SO4. The solvent was removed in vacuo to obtain 1-(2-carbomethoxyphenyl)-piperazine as a yellow oil (1.0 g, 26%).

1. temperatureThe resulting mixture was heated
2. temperatureto reflux for 7 days after which the reaction mixture
3. customThe solvent and the excess piperazine were removed in vacuo along
4. temperaturewith heating with a hot water bath
5. dissolutionThe residue was dissolved in 1N NaOH solution
6. extractionextracted with CH2Cl2 (6×30 ml)
7. dry with materialdried over Na2SO4
8. customThe solvent was removed in vacuo