HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 71269993, compound → HCID 178518792, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 71269993 | HCID 71269993 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 178518792 | HCID 178518792 | 77% |
Reaction Steps
To a degassed solution of 6-benzyl-3,4-bis(benzyloxy)pyridazine (Intermediate 23: 0.16 g, 0.418 mmol) in methanol (4.18 ml) was added 10% palladium on carbon (0.045 g, 0.042 mmol). The mixture was degassed, evacuated and filled with hydrogen from a balloon. After 1 hour the reaction mixture was degassed and filtered through a pad of “Celite” diatomaceous earth, washing with methanol and concentrated to give a yellow oil. The crude oil was purified by reverse phase chromatography (25 g C18) cartridge eluting with 5-100% acetonitrile/water with acidic modifier and the appropriate fractions combined to give a cream solid (yield=77%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09290456B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-f06d3d07976b490c8bc246f071bf09d1 |
| Source note | uspto-grants-2016_03 |