反应详情

A solution of 3,8-diaza-bicyclo[3.2.1]octane-8-carboxylic acid tert-butyl ester (2.5 g, 11.7 mmol) in CH2Cl2 (50 mL) was treated with trimethylsilyl isocyanate (14 mL, 117 mmol). The resultant mixture was stirred at rt for 4 h., concentrated and redissolved in CH2Cl2 (50 mL). To this solution was added HCl (4.0 N in 1,4-dioxane, 12 mL), and the resultant mixture was stirred at rt for 3 h. Concentration afforded the title compound as a white powder (2.4 g, 99%). MS (ESI): mass calcd. for C7H13N3O, 155.1; m/z found, 156.2 [M+H]+.

1. concentrationconcentrated
2. dissolutionredissolved in CH2Cl2 (50 mL)
3. additionTo this solution was added HCl (4.0 N in 1,4-dioxane, 12 mL)
4. concentrationConcentration