反应详情

(3R,5S)-1-(tert-Butoxycarbonyl)-5-[({2-tert-butyl-4-[(3-methoxypropyl)amino]pyrimidin-5-yl}carbonyl)(isobutyl)amino]piperidine-3-carboxylic acid (102 mg), (2R)-2-(methoxymethyl)pyrrolidine (64 mg), HOBt (20 mg) and triethylamine (104 μl) were dissolved in DMF (5 ml), WSC.HCl (107 mg) was added, and the mixture was stirred at room temperature for 18 hr. The reaction mixture was concentrated under reduced pressure, and diluted with saturated aqueous sodium hydrogen carbonate, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous magnesium 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 (0:1-1:0) was concentrated under reduced pressure to give the object compound (91 mg).

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. additiondiluted with saturated aqueous sodium hydrogen carbonate
3. extractionthe mixture was extracted with ethyl acetate
4. washThe extract was washed with saturated brine
5. dry with materialdried over anhydrous magnesium sulfate
6. customThe solvent was evaporated under reduced pressure
7. washthe fraction eluted with ethyl acetate-hexane (0:1-1:0)
8. concentrationwas concentrated under reduced pressure