反应详情

tert-Butyl 4-(2-oxo-1,2-dihydrospiro[benzo[d][1,3]oxazine-4,4′-piperidine]-1′-yl)piperidine-1-carboxylate (vib) (432 mg, 1.08 mmol) was dissolved in 3.0 N methanolic HCl (10 mL) and stirred at room temperature for 18 hours. Additional 3.0 N methanolic HCl was added (10 mL) and the reaction heated at 60° C. for 2 hours. The reaction mixture was concentrated under reduced pressure, treated with acetonitrile (approx. 25 mL) and re-concentrated to afford 1′-(piperidin-4-yl)spiro[benzo[d][1,3]oxazine-4,4′-piperidin]-2(1H)-one (compound no. 49) bis-hydrochloride as a crystalline white solid. LC/MS m/z 302.0 [M+H]+, retention time 0.34 min (RP-C18, 10-99% CH3CN/0.05% TFA).

1. temperaturethe reaction heated at 60° C. for 2 hours
2. concentrationThe reaction mixture was concentrated under reduced pressure
3. additiontreated with acetonitrile (approx. 25 mL)
4. concentrationre-concentrated