HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrazine hydrate (1:1) → HCID 21882687, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Reactant | HCID 21882742 | HCID 21882742 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 21882687 | HCID 21882687 | 69.3% |
Reaction Steps
A mixture of 1.11 g of 2-amino-4-(2-phenylethoxy)-3-nitropyridine (starting material K2), 1.0 ml of hydrazine hydrate and 0.130 g of Raney nickel in 30 ml of methanol is heated under reflux until no starting material is detectable by TLC. After filtration and evaporation of the solvent the residue is chromatographed on silica gel (dichloromethane/methanol 20:1+1% triethylamine). Concentration of the pure fractions and drying in vacuo gives 0.68 g of the title compound as an oil, which crystallizes on standing (m.p. 86–87° C.). The mass spectrum shows the molecular peak MH+ at 230.2 Da.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07138399B2 |
| Source dataset | uspto-grants-2006_11 |
| ORD ID | ord-97611bd682ff4fc384c8b68084de495e |
| Source note | uspto-grants-2006_11 |