HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 22633672, compound → HCID 22633670, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 22633672 | HCID 22633672 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Catalyst | Palladium Chloride | HCID 24290 | — |
| Solvent | tert-Butanol | HCID 6386 | — |
| Product | HCID 22633670 | HCID 22633670 | 91% |
Reaction Steps
6-Bromo-9,9-dimethyl-3-oxo-1,2,3,9,10,10a-hexahydrophenanthrene (0.250 g, 0.819 mmol)), palladium(II) dichloride (0.190 g, 10.7 mmol) and tert-butanol (5 ml) were mixed in a sealed tube and heater to 125-135° C. for 4 hours. The reaction is finished when all the palladium has precipitated on the glass wall and a yellow and transparent reaction mixture is observed. Water was then added and the aqueous phase was extracted with ethyl acetate. The organic extracts were dried with anhydrous magnesium sulfate and concentrated. The residue was purified by silica gel chromatography (ethyl acetate/hexane 5:95 to 10:90) to give the title material (0.225 g, 91%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06825233B2 |
| Source dataset | uspto-grants-2004_11 |
| ORD ID | ord-f102f6240a4b4a7591c51db48b6e4c1b |
| Source note | uspto-grants-2004_11 |