反应详情

(±)-trans-benzyl 3-(tert-butoxycarbonylamino)-4-(cyclobutylmethyl)piperidine-1-carboxylate (14 mg, 0.035 mmol)) was dissolved in 1:1 2N aq HCl/acetonitrile (8 mL) and stirred overnight at rt. 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 (±)-trans-benzyl 3-amino-4-(cyclobutylmethyl)piperidine-1-carboxylate (8.9 mg, 85% yield). The crude product was used in the next step without further purification. MS ESI +ve m/z 303 (M+Na).

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