HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 86753394, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | 2,2-Diethoxyethylamine | HCID 69524 | — |
| Reactant | HCID 22105989 | HCID 22105989 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 86753394 | HCID 86753394 | 54.1% |
Reaction Steps
A solution of 2-hydroxy-N-[α-(3-amino-4-pyridyl)-2-chlorobenzylidene]-ethylamine (6.28 g, 22 mmol), aminoacetaldehyde diethyl acetal (10 g, 75.1 mmol) and acetic acid (3 ml) in ethanol (150 ml) was refluxed for 30 hours. The mixture was concentrated under reduced pressure, and to the residue was added water, and the mixture was extracted with ethyl acetate. The extract was washed with water, washed with a saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was purified by column chromatography (silica gel; methanol: chloroform=1:9) to give the title compound (4.27 g, 11.9 mmol) as a pale yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05843957 |
| Source dataset | uspto-grants-1998_12 |
| ORD ID | ord-308cbb4c25aa42138e0e467bff3d97d4 |
| Source note | uspto-grants-1998_12 |