HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 86632977, compound → HCID 16123879, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 86632977 | HCID 86632977 | — |
| Reactant | HCID 178477796 | HCID 178477796 | — |
| Catalyst | HCID 178506421 | HCID 178506421 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 16123879 | HCID 16123879 | — |
Reaction Steps
The title compound was prepared by treating the product from step (ii) (0.25 g) in dry dioxane (10 ml) with bisdiphenylphosphinoferrocene palladium (0.02 g) and 2.0M dimethylzinc in toluene (0.40 ml). The mixture was heated to reflux for 3 h, partitioned between water and ethyl acetate, the organics separated, dried (MgSO4) and evaporated under reduced pressure to an oil. The oil was dissolved in methanol (10 ml), 2M NaOH (10 ml) added and stirred at RT overnight. The mixture was diluted with water, extracted with ether (discarded). The aqueous layer was acidified with 2M HCl, extracted with ethyl acetate, dried (MgSO4) and evaporated under reduced pressure to an oil, which was purified by RPHPLC to give a white solid (0.085 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08148572B2 |
| Source dataset | uspto-grants-2012_04 |
| ORD ID | ord-7c99c5fff31d45da8e51c5df92561e45 |
| Source note | uspto-grants-2012_04 |