反应详情

温度

110 °C

A mixture of 2-bromo(methylsulfonyl)benzene (1.10 g, 4.7 mmol) and anhydrous piperazine (2.02 g, 23.5 mmol) was heated at 110° C. overnight. Then, the mixture was cooled and partitioned between 2 N NaOH and CH2Cl2. The separated organic layer was dried over Na2SO4 and concentrated under reduced pressure. The crude residue was chromatographed (CHCl3/CH3OH, 9:1, as eluent) to give 8 as a white semisolid (0.36 g, 34% yield). 1H NMR: δ 2.58 (s, 1H, NH, D2O exchanged), 2.84 (s, 4H, piperazinic), 3.14 (s, 3H, CH3), 7.10-7.83 (m, 4H, aromatic).

1. temperatureThen, the mixture was cooled
2. custompartitioned between 2 N NaOH and CH2Cl2
3. dry with materialThe separated organic layer was dried over Na2SO4
4. concentrationconcentrated under reduced pressure
5. customThe crude residue was chromatographed (CHCl3/CH3OH, 9:1, as eluent)