反应详情

To a solution of (S)-tert-butyl 1-(6-fluoro-1-phenyl-1H-benzo[d]imidazol-2-yl)propylcarbamate (234 mg, 0.63 mmol) in DCM (3 mL) was added TFA (1.5 mL) and the mixture was stirred at RT for 2 h. Volatiles were removed under reduced pressure and the resulting residue was partitioned between DCM (20 mL) and a saturated solution of NaHCO3. The two phase system was stirred for 10 min, then the organic layer was dried (MgSO4) and concentrated in vacuo. The resulting residue was purified by column chromatography (Si—PCC, gradient 0-10% MeOH in DCM) affording (S)-1-(6-fluoro-1-phenyl-1H-benzo[d]imidazol-2-yl)propan-1-amine as a colourless oil (42 mg, 25%). LCMS: RT 1.90 min [M−NH2] 253.0

1. customVolatiles were removed under reduced pressure
2. customthe resulting residue was partitioned between DCM (20 mL)
3. stirringThe two phase system was stirred for 10 min
4. dry with materialthe organic layer was dried (MgSO4)
5. concentrationconcentrated in vacuo
6. customThe resulting residue was purified by column chromatography (Si—PCC, gradient 0-10% MeOH in DCM)