HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 67800901, compound → HCID 67801453, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 67800901 | HCID 67800901 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 67801453 | HCID 67801453 | 49.4% |
Reaction Steps
The compound obtained in Example 228 (680 mg, 2.0 mmol) was dissolved in water (30 ml). To the obtained solution, 10% palladium-on-carbon (600 mg) was added, followed by stirring at 80° C. for 10 hours in the atmosphere of hydrogen. The reaction mixture was filtered, and the filtrate was condensed under reduced pressure. The resultant residue was purified by silica gel column chromatography (chloroform: methanol =5:1). The obtained crystals were dissolved in methanol (5 ml), and 4N-HCl dioxane (1 ml) was added thereto while cooling on ice. The mixture was condensed under reduced pressure. The resultant residue was recrystallized from methanol--ether, to obtain 300 mg of the title compound as colorless powdery crystals (44.1%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05576324 |
| Source dataset | uspto-grants-1996_11 |
| ORD ID | ord-c8ebc09f51524d39a7af6da5c4357beb |
| Source note | uspto-grants-1996_11 |