HuagongsheHuagongshe Chemistry Print Report · For research reference only
Binap, (A+-)- → (3R)-3-methyl-1-(1H,3H-naphtho[1,8-cd]pyran-6-yl)piperazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Binap, (A+-)- | HCID 634876 | — |
| Reactant | 2-Methylpiperazine, (R)- | HCID 7330434 | — |
| Reactant | Sodium t-butoxide | HCID 23676156 | — |
| Reactant | 6-bromo-1H,3H-naphtho[1,8-cd]pyran | HCID 69307283 | — |
| Catalyst | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | (3R)-3-methyl-1-(1H,3H-naphtho[1,8-cd]pyran-6-yl)piperazine | HCID 69306502 | — |
Reaction Steps
A mixture of 6-bromo-1H,3H-naphtho[1,8-cd]pyran (0.30 g, 1.2 mmol), 2-(R)-methylpiperazine (0.145 g, 1.44 mmol), tris(dibenzylideneacetone)dipalladium(0) (55 mg, 0.06 mmol), rac-2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (56 mg, 0.09 mmol) and sodium tert-butoxide (0.162 g, 1.68 mmol) in toluene (5 mL) was heated under reflux for 2 h. The solvent was evaporated in vacuo and the crude mixture purified by column chromatography on silica gel, eluting with dichloromethane/methanol (9:1), to yield (3R)-3-methyl-1-(1H,3H-naphtho[1,8-cd]pyran-6-yl)piperazine as an orange solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07335660B2 |
| Source dataset | uspto-grants-2008_02 |
| ORD ID | ord-3246601d97494adcb52ff263b8e80177 |
| Source note | uspto-grants-2008_02 |