反应详情

1-(1-Methyl-4-piperidinyl)piperazine (1.126 mmol) was dissolved in methylene chloride (7 ml), the solution was cooled in an ice bath and triethylamine (2.8 mmol) and (1-(3-(trifluoromethyl)phenylsulfonyl)piperidin-2-yl)methanesulfonic acid chloride (dissolved in methylene chloride (3 ml)) were added. The mixture was stirred for 16 h, during which it was allowed to warm slowly to room temperature. The reaction mixture was diluted with methylene chloride and washed with water and the organic phase was dried over sodium sulfate and concentrated in vacuo. The crude product was purified by column chromatography (silica gel) with methylene chloride/methanol (19:1). Yield: 30%. MS, Rt=2.4 min, m/z=553.0 [MH]+

1. temperaturethe solution was cooled in an ice bath
2. washwashed with water
3. dry with materialthe organic phase was dried over sodium sulfate
4. concentrationconcentrated in vacuo
5. customThe crude product was purified by column chromatography (silica gel) with methylene chloride/methanol (19:1)