反应条件: temp:110.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 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).
Then, the mixture was cooled
partitioned between 2 N NaOH and CH2Cl2
The separated organic layer was dried over Na2SO4
concentrated under reduced pressure
The crude residue was chromatographed (CHCl3/CH3OH, 9:1, as eluent)
来源 ID: ord-f2fa2b6266a2460a97f9d62d6a21fa0a