反应详情

(3S,4S)-benzyl 3-(tert-butoxycarbonylamino)-4-cyclohexylpiperidine-1-carboxylate (35 mg, 0.084 mmol) was dissolved in 1:1 2N aq HCl/acetonitrile (8 mL) and stirred overnight at rt. LC-MS showed the reaction was complete. The reaction mixture was basified with 5% aq NaOH solution to about pH=9. The acetonitrile was removed under vacuum. The aqueous residue was extracted with CH2Cl2 (3×20 mL). The combined organic layers were washed with brine (10 mL) and dried over Na2SO4. Concentration afforded (3S,4S)-benzyl 3-amino-4-cyclohexylpiperidine-1-carboxylate (23 mg, 86% yield). The crude product was used in the next step without further purification. LC-MS (3 min) tR=1.31 min., m/z 317 (M+1).

1. customThe acetonitrile was removed under vacuum
2. extractionThe aqueous residue was extracted with CH2Cl2 (3×20 mL)
3. washThe combined organic layers were washed with brine (10 mL)
4. dry with materialdried over Na2SO4
5. concentrationConcentration