HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,3-Diaminopyridine → HCID 22711785, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,3-Diaminopyridine | HCID 9956 | — |
| Reactant | HCID 22711787 | HCID 22711787 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 22711785 | HCID 22711785 | 52.7% |
Reaction Steps
A mixture of 2,3-pyridinediamine (0.05 mol) and ethyl 4-(2-ethoxy-2-iminoethyl)-1-piperidinecarboxylate monohydrochloride (0.05 mol) in methanol (150 ml) was stirred and refluxed for 3 days. The solvent was evaporated and the residue was taken up in CH2Cl2. The organic solution was washed with K2CO3 10%, dried, filtered and the solvent was evaporated. The residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH/NH4OH 94/6/0.1). The pure fractions were collected and the solvent was evaporated, yielding 7.6 g of ethyl 4-[(1H-imidazo[4,5-b]pyridin-2-yl)methyl]-1-piperidinecarboxylate (52%) (interm. 9).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07528149B2 |
| Source dataset | uspto-grants-2009_05 |
| ORD ID | ord-0bfe039519f8454c9d684a858f54ab23 |
| Source note | uspto-grants-2009_05 |