反应详情

A solution of (3R,5S)-1-(tert-butoxycarbonyl)-5-[({2-tert-butyl-4-[(3-methoxypropyl)amino]pyrimidin-5-yl}carbonyl)(isobutyl)amino]piperidine-3-carboxylic acid (95 mg), WSC.HCl (50 mg), HOBt (34 g) and diisopropylethylamine (0.088 ml) in DMF (5 ml) was stirred at room temperature for 12 hr. The reaction mixture was poured into saturated aqueous sodium hydrogen carbonate, and the mixture was extracted with ethyl acetate. The extract was washed successively with 10% aqueous citric acid solution and saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The residue was subjected to silica gel column chromatography, and the fraction eluted with ethyl acetate-hexane (1:1-1:0) was concentrated under reduced pressure to give an amorphous solid (65 mg).

1. extractionthe mixture was extracted with ethyl acetate
2. washThe extract was washed successively with 10% aqueous citric acid solution and saturated brine
3. dry with materialdried over anhydrous sodium sulfate
4. customThe solvent was evaporated under reduced pressure
5. washthe fraction eluted with ethyl acetate-hexane (1:1-1:0)
6. concentrationwas concentrated under reduced pressure