反应详情

To an ice-cooled solution of 2,2-dimethylpropionic acid 2-{(S)-3-[2-((S)-2-tert-butoxycarbonylaminopropionylamino)-5-fluorophenylamino]piperidin-1-yl}ethyl ester (2.054 g, 4.04 mmol) in DCM (40 mL) was added TFA (14 mL) and the mixture stirred at RT for 1.5 h. Toluene was added and the volatiles removed in vacuo. The resulting residue was dissolved in MeOH and loaded onto an Isolute® SCX-2 cartridge. The cartridge was washed with MeOH and the product eluted with 0.5M NH3/MeOH. The product containing fractions were combined and concentrated in vacuo. The resulting residue was purified by column chromatography (Si—PCC, gradient 2-10% 2M NH3/MeOH in DCM) affording the title compound as a purple oil (1.443 g, 87%). LCMS (Method B): RT 1.60 min [M+H]+ 409.

1. customthe volatiles removed in vacuo
2. dissolutionThe resulting residue was dissolved in MeOH
3. washThe cartridge was washed with MeOH
4. washthe product eluted with 0.5M NH3/MeOH
5. additionThe product containing fractions
6. concentrationconcentrated in vacuo
7. customThe resulting residue was purified by column chromatography (Si—PCC, gradient 2-10% 2M NH3/MeOH in DCM)