反应详情

4N HCl in dioxane (3.29 mL, 13.2 mmol) was added to a solution of cis-tert-butyl 3-(benzyloxycarbonylamino)-4-fluoropiperidine-1-carboxylate (0.58 g, 1.65 mmol) in DCM (3 mL) at room temperature. The reaction mixture was stirred at room temperature for 2 hours. The solvent was removed in vacuo. The resulting solid was dissolved in water (5 mL) and extracted with ether (10 mL). The resulting aqueous layer was basified with 30% potassium carbonate to a pH of about 10 and extracted with DCM (2×30 mL). The combined organic layer was dried (sodium sulfate) and concentrated in vacuo to give benzyl-cis-4-fluoropiperidin-3-ylcarbamate (0.39 g, 94%) as a solid.

1. customThe solvent was removed in vacuo
2. dissolutionThe resulting solid was dissolved in water (5 mL)
3. extractionextracted with ether (10 mL)
4. extractionextracted with DCM (2×30 mL)
5. dry with materialThe combined organic layer was dried (sodium sulfate)
6. concentrationconcentrated in vacuo