反应详情

温度

90 °C

4-(3-Methanesulfonyloxy-propyl)-benzoic acid methyl ester (800 mg, 2.9 mmol), piperidin-3-yl-carbamic acid tert-butyl ester (290 mg, 1.45 mmol), potassium carbonate (500 mg, 3.6 mmol) and sodium iodide (100 mg 0.67 mmol) in acetonitrile (20 ml) are heated under reflux for two days and evaporated. The residue is taken up in dimethylsulfoxide (10 ml) and stirred at 90° C. for 5 h. The resulting mixture is purified by preparative HPLC-MS (MeOH/H2O+0.1% TFA). Potassiumcarbonate solution is added to the product, extracted with ethyl acetate, the organic phase is dried over Na2SO4 and concentrated in vacuo. LC (method F): tR=1.66 min; Mass spectrum (ESI+): m/z=377 [M+H]+.

1. temperatureunder reflux for two days
2. customevaporated
3. customThe resulting mixture is purified by preparative HPLC-MS (MeOH/H2O+0.1% TFA)
4. additionPotassiumcarbonate solution is added to the product
5. extractionextracted with ethyl acetate
6. dry with materialthe organic phase is dried over Na2SO4
7. concentrationconcentrated in vacuo