反应详情

A stirred solution of aniline (15.3 g, 0.16 mol) and di-isopropyl ethylamine (DIEA, 56 mL, 0.33 mol) in acetonitrile (120 mL) is heated to 60° C. and 2-chloro-1-(4-(naphthalen-2-ylsulfonyl)piperazin-1-yl)ethanone (compound 5, 0.3 g, 0.85 mmol) is added dropwise. The reaction mixture is kept stirring at this temperature for another 3 h and is then evaporated to dryness. Water is added to the residue, and extracted with ethyl acetate (2×30 mL). The organic extract was dried over anhydrous sodium sulphate, filtered and concentrated under reduced pressure. The resultant crude product was purified by column chromatography on silica gel (hexane:ethyl acetate:3:7) to obtain the title compound (300 mg, 76.53%) as an off-white solid.

1. customis then evaporated to dryness
2. additionWater is added to the residue
3. extractionextracted with ethyl acetate (2×30 mL)
4. extractionThe organic extract
5. dry with materialwas dried over anhydrous sodium sulphate
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. customThe resultant crude product was purified by column chromatography on silica gel (hexane:ethyl acetate:3:7)