HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 14459483, compound → HCID 14459488, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 14459483 | HCID 14459483 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 14459488 | HCID 14459488 | 51% |
Reaction Steps
3.0 g (10.3 mmol) of 6-[4-(2-aminoethyl)amino-3-nitro-phenyl]-4,5-dihydro-5-methyl-3(2H)-pyridazinone in 200 ml of methanol are hydrogenated under a hydrogen pressure of 2 bar at room temperature in the presence of 0.5 g of palladium charcoal (10% Pd) until uptake of hydrogen ceases. After removal of the catalyst by filtration, the solution is concentrated by evaporation under vacuum. The residue is chromatographed on silica gel with methanol/conc. ammonia (95/5) as solvent. The main fraction is concentrated by evaporation under vacuum and the solid obtained is recrystallized from ethanol. 1.37 g (51%) of a beige coloured solid, m.p. 176°-177° C. are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04954501 |
| Source dataset | uspto-grants-1990_09 |
| ORD ID | ord-169c741266fc435ab655b58dfe0530ab |
| Source note | uspto-grants-1990_09 |