HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 66922097, compound → HCID 66922203, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 66922097 | HCID 66922097 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 66922203 | HCID 66922203 | 16.5% |
Reaction Steps
To a solution of 8.73 g of the compound of step 2 in acetic acid (180 ml) was added zinc, and the suspension was stirred at room temperature overnight. The mixture was extracted with EA, the organic layer was separated, dried over sodium sulfate, filtered and evaporated under reduced pressure. The resulting solid was dissolved in ethanol (245 ml), and palladium on activated carbon (1.75 g, 1.64 mmol, 10%) was added. The reaction mixture was hydrogenated (5.2 bar H2) at room temperature overnight. The mixture was filtered over celite, the solvent was removed under reduced pressure and the solid was purified by silica gel chromatography (EA (10 to 70%)/HEP). 870 mg of the title compound were obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08580813B2 |
| Source dataset | uspto-grants-2013_11 |
| ORD ID | ord-2b75e856c37e4706b76466c7a7db5ad2 |
| Source note | uspto-grants-2013_11 |