反应详情

To a solution of 100 mg (S)-2-({5-[2-((S)-2-(Cyclopropylmethyl-carbamoyl)-pyrrolidin-1-yl)-2-oxo-ethoxy]-1-phenyl-1H-pyrazole-3-carbonyl}-amino)-pentanedioic acid 5-tert-butyl ester in 6 ml DMF were added 28 μl DIPEA, 64 mg HATU and 29 mg (R)-2-Methyl-piperazine-1-carboxylic acid ethyl ester. After stirring for 16 h the solution was concentrated, the residue dissolved in 1.5 ml dichloromethane and treated with 560 μl TFA. After stirring for 16 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: 65 mg MS (ES+): m/e=696.

1. concentrationwas concentrated
2. dissolutionthe residue dissolved in 1.5 ml dichloromethane
3. additiontreated with 560 μl TFA
4. stirringAfter stirring for 16 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