HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cyclohexylamine → 6-Chloro-4-(cyclohexylamino)pyridine-3-carboxyamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cyclohexylamine | HCID 7965 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 4,6-Dichloropyridine-3-carboxyamide | HCID 131730931 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 6-Chloro-4-(cyclohexylamino)pyridine-3-carboxyamide | HCID 131730993 | 93% |
Reaction Steps
200 mg of 4,6-dichloropyridine-3-carboxyamide synthesized according to the method described in US2006/0217417 was dissolved in 2 mL of ethanol, to which 156 mg of cyclohexylamine and 203 mg of N,N-diisopropylethylamine were added, and heated at reflux for 8 hours. After cooling, the solvent was evaporated, and 10 mL of water was added to the residue, neutralized by adding 2 mol/L hydrochloric acid in water under ice cooling, extracted with chloroform, and the extract was dried on anhydrous sodium sulfate. The solvent was evaporated, and the residue was recrystallized from chloroform-hexane to obtain 243 mg (92%) of the title compound as colorless needle crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08575153B2 |
| Source dataset | uspto-grants-2013_11 |
| ORD ID | ord-21f32da1f4c741ab8524519e472ad27b |
| Source note | uspto-grants-2013_11 |