HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 178480253, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | 2,3-Diaminopyridine | HCID 9956 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 1-Methylpiperidine-3-carboxylic acid hydrochloride | HCID 12514711 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 178480253 | HCID 178480253 | — |
Reaction Steps
Grams 10.9 of 2,3-diaminopyridine and 17,9 g N-methylnipecotic acid hydrochloride are heated at 190° C. for 6 hours. The reaction mixture is cooled and diluted with a small amount of water, then is made alkaline to pH 10 by addition of NaOH and extraction is repeated several times with methylene chloride. The organic extracts, collected together, are evaporated to dryness. The obtained residue, is extracted several times with diethyl ether and the ethereal extracts are evaporated to dryness. The obtained residue, crystallized from acetonitrile, provides 5 g (23% of the theoretical value) 2-(1-methylpiperidin-3-yl)-3H-imidazo-[4,5-b] pyridine melting at 141°-144° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05071855 |
| Source dataset | uspto-grants-1991_12 |
| ORD ID | ord-a3cf8bb32ef941abb73694918d4634d7 |
| Source note | uspto-grants-1991_12 |