HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 19770728, compound → HCID 19770729, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 19770728 | HCID 19770728 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 19770729 | HCID 19770729 | 90% |
Reaction Steps
A solution of 3-nitro-5-ethyl-6-benzyloxymethyl-2(1H)-pyridinone (576 mg, 2.0 mmol) in tetrahydrofuran (15 mL) and methanol (15 mL) containing 10% palladium/charcoal (130 mg) was hydrogenated at atomspheric pressure, monitoring the progress by thin layer chromatography (tlc). Additional catalyst was added in 100 mg portions after day 2 and day 3. After 3-4 days, the catalyst was filtered and the solvents evaporated. The catalyst was vigorously washed with methanol/chloroform and combined solvents evaporated. The residue was triturated with methylene chloride and productcollected by filtration to give 136 mg of 90% pure product. This material was used without further purfification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05169769 |
| Source dataset | uspto-grants-1992_12 |
| ORD ID | ord-7a15f18a3cc049298b82ecbc8ac052bb |
| Source note | uspto-grants-1992_12 |