反应详情

To a solution of 200 mg 4-[(S)-4-tert-butoxycarbonyl-2-({5-[2-(3-carboxy-pyrrolidin-1-yl)-2-oxo-ethoxy]-1-phenyl-1H-pyrazole-3-carbonyl}-amino)-butyryl]-piperazine-1-carboxylic acid ethyl ester in 5 ml DMF were added 48 μl DIPEA, 11 mg HATU and 20 μl cyclopropylamine. After stirring for 12 h saturated aqueous NaHCO3 solution was added and the mixture loaded on a Chem Elut® cartridge, the crude product being eluted with dichloromethane. The solution was concentrated to a volume of 5 ml and stirred in the presence of 324 μl TFA. After stirring for 14 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: 30 mg MS (ES+): m/e=668.

1. additionwas added
2. washthe crude product being eluted with dichloromethane
3. concentrationThe solution was concentrated to a volume of 5 ml
4. stirringAfter stirring for 14 h the solvents
5. customwere removed under reduced pressure
6. customthe residue purified by preparative HPLC (
7. washC18 reverse phase column, elution with a water/MeCN gradient with 0.1% TFA)
8. additionThe fractions containing the product
9. customto yield the pure product