HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 86633378, compound → HCID 86633377, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 86633378 | HCID 86633378 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86633377 | HCID 86633377 | — |
Reaction Steps
To a solution of the compound (9) (28.7 g, 33.3 mmol) in ethanol (400 ml) and dichloromethane (150 ml) was added 10% palladium activated carbon (7.00 g), and the mixture was stirred at room temperature for 48 hours in a hydrogen gas atmosphere. After the sufficient progress of the reaction was confirmed, palladium activated carbon was removed by filtration, and the filtrate was concentrated under reduced pressure. The obtained residue was purified with silica gel chromatography (dichloromethane-methanol, 10:1→5:1→3:1→2:1→1:1), and precipitated from 98% heated ethanol to obtain the title compound (10) in the form of a colorless powder {15.6 g (26.4 mmol), 79.4%}.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07973145B2 |
| Source dataset | uspto-grants-2011_07 |
| ORD ID | ord-30f3ba303eec4e5e8dd2cf372180b6f7 |
| Source note | uspto-grants-2011_07 |