反应详情

温度

100 °C

A mixture of tert-butyl 2-amino-4-chlorophenyl(3-(methylsulfonyl)propyl)carbamate (320 mg, 0.92 mmol) and sodium chloroacetate (130 mg, 1.1 mmol) in 4 N HCl was heated to 100° C. After overnight stirring, the reaction solution was cooled to RT and concentrated. The residue was diluted with DCM (100 mL) and washed with sat. NaHCO3 (50 mL). The organic layer was dried and concentrated under vacuum. The residue was purified by prep-TLC (DCM/EtOAc=3:1) to give 5-chloro-2-(chloromethyl)-1-(3-(methylsulfonyl)propyl)-1H-benzo[d]imidazole (130 mg, yield: 44%) as pale solid. MS obsd. (ESI+) [(M+H)+]: 321.0.

1. temperaturethe reaction solution was cooled to RT
2. concentrationconcentrated
3. additionThe residue was diluted with DCM (100 mL)
4. washwashed with sat. NaHCO3 (50 mL)
5. customThe organic layer was dried
6. concentrationconcentrated under vacuum
7. customThe residue was purified by prep-TLC (DCM/EtOAc=3:1)