反应详情

To a solution of 303 mg (S)-2-({5-[2-((S)-2-cyclobutylcarbamoyl-pyrrolidin-1-yl)-2-oxo-ethoxy]-1-phenyl-1H-pyrazole-3-carbonyl}-amino)-pentanedioic acid 5-tert-butyl ester in 5 ml DMF were added 34 μl DIPEA, 193 mg HATU and 103 mg pyrrolidin-3-yl-carbamic acid butyl ester. After stirring for 12 h the reaction mixture was diluted with ethyl acetate, washed with aqueous LiCl (4%) and saturated aqueous NaHCO3 solution. The solution was concentrated, dissolved in 2 ml dichloromethane and stirred in the presence of 384 μl TFA. After stirring for 4 h the solvents were removed under reduced pressure and the residue purified by preparative HPLC (C18 reverse phase column, elution with a water/MeCN gradient with 0.1% TFA). The fractions containing the product were lyophilized to yield the pure product. Yield: 229 mg MS (ES+): m/e=710.

1. washwashed with aqueous LiCl (4%) and saturated aqueous NaHCO3 solution
2. concentrationThe solution was concentrated
3. dissolutiondissolved in 2 ml dichloromethane
4. stirringstirred in the presence of 384 μl TFA
5. stirringAfter stirring for 4 h the solvents
6. customwere removed under reduced pressure
7. customthe residue purified by preparative HPLC (
8. washC18 reverse phase column, elution with a water/MeCN gradient with 0.1% TFA)
9. additionThe fractions containing the product
10. customto yield the pure product