反应详情

Benzyl 3-(tert-butoxycarbonylamino)piperidine-1-carboxylate (1 g, 2.99 mmol) was treated with Dioxane.HCl (30 mL) at 0° C. The reaction mixture was stirred at rt for 1 h. After completion of the reaction mixture, the solvent was removed under vacuo and the residue was dissolved in H2O (10 mL). The aqueous layer was treated with solid Na2CO3 until effervescence ceases and the solution was extracted with EtOAc (3×25 mL). The combined organic layer was dried over Na2SO4, concentrated to yield titled intermediate (700 mg, 92%), which was used in the next step without further purification. 1H NMR (400 MHz, DMSO-d6): δ 7.41-7.25 (m, 5H), 5.08 (s, 2H), 3.95-3.78 (m, 2H), 3.22 (bs, 2H), 2.82-2.75 (m, 1H), 2.61-2.45 (m, 2H), 1.82-1.78 (m, 1H), 1.69-1.59 (m, 1H), 1.40-1.33 (m, 1H), 1.22-1.10 (m, 1H). ES-MS: m/z [M+1]=235.

1. customat 0° C
2. customAfter completion of the reaction mixture, the solvent was removed under vacuo
3. dissolutionthe residue was dissolved in H2O (10 mL)
4. additionThe aqueous layer was treated with solid Na2CO3 until effervescence ceases
5. extractionthe solution was extracted with EtOAc (3×25 mL)
6. dry with materialThe combined organic layer was dried over Na2SO4
7. concentrationconcentrated