HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 59258500, compound → 1'-(piperidin-4-yl)spiro[benzo[d][1,3]oxazine-4,4'-piperidin]-2(1H)-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 59258500 | HCID 59258500 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Product | 1'-(piperidin-4-yl)spiro[benzo[d][1,3]oxazine-4,4'-piperidin]-2(1H)-one | HCID 25060956 | — |
Reaction Steps
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).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07696201B2 |
| Source dataset | uspto-grants-2010_04 |
| ORD ID | ord-a091f99680594aedac35852f7967dc98 |
| Source note | uspto-grants-2010_04 |