反应详情

20 g (84.5 mmol) diphenylphosphinate chloride dissolved in 30 ml DMF are added dropwise to a solution of 21.8 g (253 mmol) piperazine in DMF. After four hours, the solution is concentrated under vacuum, taken up in chloroform and extracted by shaking with 10% hydroxide solution. The organic phase is dried over sodium sulfate and solvent is removed under vacuum. The residue is chromatographically purified over silica gel with CHCl3/CH3OH/TEA (90/10/0 to 90/10/6): yield 12 g (49%).

1. concentrationthe solution is concentrated under vacuum
2. extractionextracted
3. dry with materialThe organic phase is dried over sodium sulfate and solvent
4. customis removed under vacuum
5. customThe residue is chromatographically purified over silica gel with CHCl3/CH3OH/TEA (90/10/0 to 90/10/6)