反应详情

A solution of [(S)-1-(2-chloro-6-phenylaminophenylcarbamoyl)ethyl]carbamic acid tertbutyl ester (1.58 g, 4.05 mmol) in AcOH (25 mL) was stirred for 18 h at 65° C. After cooling to RT, volatiles were evaporated under reduced pressure and the residue was partitioned between EtOAc and a saturated solution of NaHCO3. The aqueous phase was further extracted with EtOAc and the combined organic layers were washed with brine, then dried (Na2SO4) and concentrated in vacuo. The resulting residue was purified by column chromatography (Si—PCC, gradient 0-2% 2M NH3/MeOH in DCM) affording [(S)-1-(4-Chloro-1-phenyl-1H-benzoimidazol-2-yl)ethyl]carbamic acid tertbutyl ester as an off-white solid (1.41 g, 93%). LCMS: RT 3.90 min [M+H]+ 372.2.

1. customvolatiles were evaporated under reduced pressure
2. customthe residue was partitioned between EtOAc
3. extractionThe aqueous phase was further extracted with EtOAc
4. washthe combined organic layers were washed with brine
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated in vacuo
7. customThe resulting residue was purified by column chromatography (Si—PCC, gradient 0-2% 2M NH3/MeOH in DCM)