HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyrrolidine → tert-Butyl 6-bromo-4-oxospiro[chroman-2,4'-piperidine]-1'-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyrrolidine | HCID 31268 | — |
| Reactant | 5'-Bromo-2'-hydroxyacetophenone | HCID 95991 | — |
| Reactant | tert-Butyl 4-oxopiperidine-1-carboxylate | HCID 735900 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | tert-Butyl 6-bromo-4-oxospiro[chroman-2,4'-piperidine]-1'-carboxylate | HCID 2794759 | 94% |
Reaction Steps
A mixture of 2-hydroxy-5-bromoacetophenone (10.75 g, 50 mmol), N—BOC-4-piperidone (9.96 g, 50 mmol) and pyrrolidine (2.09 ml, 25 mmol) in MeOH (80 ml) was heated to reflux for 11 h. The solvent was removed under vacuum and the crude mixture was purified by column chromatography (eluent: hexane/AcOEt 90:10 to 80:20) to give 6-bromo-4-oxo-spiro[chromane-2,4′-piperidine]-1′-carboxylic acid tert-butyl ester (18.55 g) as a yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09115148B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-53e9ed24be7f4a63b4e09f54f05a9a4e |
| Source note | uspto-grants-2015_08 |