HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → 1-(3-Methyl[1,2,4]triazolo[4,3-a]pyridin-6-yl)cyclopropanecarboxylic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Acetaldehyde | HCID 177 | — |
| Reactant | Iodo benzene diacetate | HCID 12217721 | — |
| Reactant | Methyl 1-(6-hydrazinopyridin-3-yl)cyclopropanecarboxylate | HCID 59216299 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 1-(3-Methyl[1,2,4]triazolo[4,3-a]pyridin-6-yl)cyclopropanecarboxylic acid | HCID 59216287 | 30.3% |
Reaction Steps
To a solution of methyl 1-(6-hydrazinopyridin-3-yl)cyclopropanecarboxylate (150 mg, 0.72 mol) in ethanol (3 mL) was added acetaldehyde (33.5 mg, 0.760 mmol) and acetic acid (41 μL, 0.72 mmol). The mixture was stirred at RT for 2 h, and then concentrated to dryness. The residue was dissolved in methylene chloride (3 mL), and iodobenzene diacetate (256 mg, 0.796 mmol) was added dropwise. The reaction mixture was stirred at RT overnight. The reaction solution was concentrated to dryness. The residue was purified through silica gel chromatograph using 10% MeOH in CH2Cl2 to afford the desired compound (50 mg, 30%). Analytical LCMS: (M+H)+=218.0.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08143251B2 |
| Source dataset | uspto-grants-2012_03 |
| ORD ID | ord-6cbe1eab8f8b4dfcaf54b1625b540d60 |
| Source note | uspto-grants-2012_03 |