HuagongsheHuagongshe Chemistry Print Report · For research reference only
5-Bromoacenaphthene → (3R)-1-(1,2-Dihydro-5-acenaphthylenyl)-3-methylpiperazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 5-Bromoacenaphthene | HCID 74923 | — |
| Reactant | Binap, (A+-)- | HCID 634876 | — |
| Reactant | 2-Methylpiperazine, (R)- | HCID 7330434 | — |
| Reactant | Sodium t-butoxide | HCID 23676156 | — |
| Catalyst | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | (3R)-1-(1,2-Dihydro-5-acenaphthylenyl)-3-methylpiperazine | HCID 69307361 | — |
Reaction Steps
A mixture of 2-(R)-methylpiperazine (0.124 g, 1.1 mmol), tris(dibenzylideneacetone)dipalladium(0) (49 mg, 0.05 mmol), rac-2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (69 mg, 0.10 mmol) and sodium tert-butoxide (0.148 g, 1.5 mmol) were stirred in toluene (50 mL) under nitrogen for 15 min to give a blood red solution. 5-Bromo-1,2-dihydroacenaphthylene (0.256 g, 1.1 mmol) was added, the solution stirred under nitrogen and heated at reflux for 3 h. The mixture was cooled, diluted with dichloromethane and filtered through celite. The organic phase was washed with water, dried (MgSO4), filtered and evaporated in vacuo. The crude product was taken forward to the next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07335660B2 |
| Source dataset | uspto-grants-2008_02 |
| ORD ID | ord-a244e5c7cab34822b5f2eb0206c39364 |
| Source note | uspto-grants-2008_02 |