HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → HCID 67446904, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Ammonium formate | HCID 2723923 | — |
| Reactant | 4-Chloro-2-(4-methoxybenzyl)-5-morpholinopyridazin-3(2H)-one | HCID 67446490 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 67446904 | HCID 67446904 | — |
Reaction Steps
To a mixture of 4-chloro-2-(4-methoxybenzyl)-5-(morpholin-4-yl)pyridazin-3(2H)-one (8.56 g, 25.50 mmol) and 10% Pd/C catalyst (1.45 g) in methanol (105 ml) was added ammonium formate (3.70 g, 58.7 mmol), and the mixture was refluxed under argon with TLC monitoring (ethyl acetate). Further portions of ammonium formate were added until the starting material was completely consumed. The catalyst was filtered off and washed with methanol, then the solvent was evaporated under reduced pressure. The residue was taken up in water (30 ml) and extracted with dichloromethane (4×40 ml). The combined extracts were washed with water, dried (Na2SO4) and evaporated. The crude product was purified by crystallization from ethanol (95%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08536210B2 |
| Source dataset | uspto-grants-2013_09 |
| ORD ID | ord-70c7a501a0ad4ab782260a29eb67f388 |
| Source note | uspto-grants-2013_09 |