反应详情

温度

65 °C

1.17 g (4.85 mmol) of 1-(4-bromophenyl)piperazine are added to a solution of 1.47 g (4 mmol) of 2-(methylamino)-2-oxoethyl 4-nitrophenyl carbonate, obtained in step 2.1, in 18 ml of 1,2-dichloroethane. This reaction mixture is heated at 65° C. for 2.25 hours. The mixture is allowed to cool to room temperature and it is then concentrated under reduced pressure. The oily yellow residue is taken up in dichloromethane and washed successively with sodium hydroxide (1N), water, aqueous 5% citric acid solution, water and then brine. This organic phase is dried over sodium sulfate and is concentrated under reduced pressure. After washing with diisopropyl ether, 1.3 g of product are obtained in the form of a white solid.

1. temperatureto cool to room temperature
2. concentrationit is then concentrated under reduced pressure
3. washwashed successively with sodium hydroxide (1N), water, aqueous 5% citric acid solution, water
4. dry with materialThis organic phase is dried over sodium sulfate
5. concentrationis concentrated under reduced pressure
6. washAfter washing with diisopropyl ether, 1.3 g of product
7. customare obtained in the form of a white solid