反应详情

t-Butyl trans-4-aminomethylcyclohexylcarbamate (344 mg, 1.5 mmol) was dissolved in CH2Cl2 (7 mL) and cooled in an ice-bath. Triethylamine (0.21 mL, 1.5 mmol) was added, followed by benzyl chloroformate (0.22 mL, 1.5 mmol) dropwise. The mixture was stirred at rt under N2 for 2 h. The reaction mixture was diluted with CH2Cl2 and washed with water and brine, dried over Na2SO4, filtered, and concentrated to a white solid. This solid was dissolved in 10 mL of 4 N HCl-dioxane and stirred at rt for 10 min. The solvent was removed. The residue was dried under vacuum to give 350 mg of the desired product as a white solid (78%). MS 263.36 (M+H)+.

1. temperaturecooled in an ice-bath
2. washwashed with water and brine
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated to a white solid
6. dissolutionThis solid was dissolved in 10 mL of 4 N HCl-dioxane
7. stirringstirred at rt for 10 min
8. customThe solvent was removed
9. customThe residue was dried under vacuum