Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Propylamine | HCID 7852 | — |
| Reactant | 2-chloro-N-(2-chloropyridin-3-yl)pyridine-3-carboxamide | HCID 2747538 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 19960061 | HCID 19960061 | — |
Reaction Steps
26.8 g (0.1 mol) of 2-chloro-N-(2-chloro-3-pyridinyl)-3-pyridinecarboxamide were dissolved in 200 ml of dioxane, and the resulting solution was admixed with 21.4 g (0.362 mol) of propylamine. Thereafter, the mixture was shaken in a stainless steel pressure vessel at 150° C. for 6 hours. The reaction mixture was then evaporated in vacuo, and the residue was purified by column chromatography on silica gel, successively using dichloromethane/ethyl acetate 10/1 (v/v) and dichloromethane/cyclohexane/ethyl acetate 1/2/1 (v/v/v) as eluents. The product obtained by evaporation was a highly viscous resin that had a satisfactory quality for the following reaction.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US05620974 |
|---|
| Source dataset | uspto-grants-1997_04 |
|---|
| ORD ID | ord-efbe71241ae747cda889e5c1422a8fdf |
|---|
| Source note | uspto-grants-1997_04 |
|---|