反应详情

1,1-Dimethylethyl (2S)-4-({4-[({4-[(3-fluorophenyl)amino]-1-piperidinyl}carbonyl)(methyl)amino]phenyl}methyl)-2-methyl-1-piperazinecarboxylate (D33) (9.337 g, 17.322 mmol) was dissolved in DCM (144 mL) and cooled in an ice bath. TFA (36 mL) was added slowly and the mixture was allowed to stir for 2.5 h under argon. The solvent was removed under vacuum and the residue partitioned between DCM and saturated aqueous NaHCO3. The organic layer was separated and the aqueous layer extracted twice with DCM. The combined organic extracts were dried and concentrated to give the title compound as a cream coloured foam (7.82 g). MS (ES): MH+ 440.3.

1. temperaturecooled in an ice bath
2. customThe solvent was removed under vacuum
3. customthe residue partitioned between DCM and saturated aqueous NaHCO3
4. customThe organic layer was separated
5. extractionthe aqueous layer extracted twice with DCM
6. customThe combined organic extracts were dried
7. concentrationconcentrated