HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Methylcyclohexanone → 6-Bromo-4'-methylspiro(chroman-2,1'-cyclohexan)-4-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Methylcyclohexanone | HCID 11525 | — |
| Reactant | Pyrrolidine | HCID 31268 | — |
| Reactant | 5'-Bromo-2'-hydroxyacetophenone | HCID 95991 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 6-Bromo-4'-methylspiro(chroman-2,1'-cyclohexan)-4-one | HCID 58424034 | 156.5% |
Reaction Steps
A mixture of 1-(5-bromo-2-hydroxy-phenyl)-ethanone (20 g, 0.093 mol), 4-methylcyclohexanone (21.31 g, 0.187 mol) and pyrrolidine (12.63 g, 0.178 mol) in methanol (400 mL) was refluxed for overnight. The reaction mixture was concentrated in vacuo, diluted with an equal volume of H2O and then added HCl until pH=1. The resulting mixture was extracted with EtOAc. The organic layer was dried over anhydrous Na2SO4, filtered, and evaporated to give 6-bromo-4′-methylspiro(chroman-2,1′-cyclohexan)-4-one (45 g, 100%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08450308B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-19973ce4e71c49c19636f6922bca341f |
| Source note | uspto-grants-2013_05 |