反应详情

A round bottom flask under nitrogen atmosphere was charged with cis-methyl 4-(2-amino-5-((triisopropylsilyloxy)methyl)phenylamino)cyclohexanecarboxylate (2.5 g, 5.75 mmol) and EtOH (23.96 mL) To this was added cyanogen bromide (0.914 g, 8.63 mmol), and the reaction mixture was stirred overnight at RT. The reaction mixture was diluted with DCM (80 mL) and washed with 1N aqueous NaOH (50 mL). The organic layer was collected, dried over sodium sulfate, and concentrated to dryness to afford cis-methyl 4-(2-amino-6-((triisopropylsilyloxy)methyl)-1H-benzo[d]imidazol-1-yl)cyclohexanecarboxylate as a brown solid (2.64 g, 100% yield). MS m/z=460.2 [M+H]. Calc'd for C25H41N3O3Si: 459.3.

1. washwashed with 1N aqueous NaOH (50 mL)
2. customThe organic layer was collected
3. dry with materialdried over sodium sulfate
4. concentrationconcentrated to dryness