HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,1,1-Trifluoro-2,4-pentanedione → Methyl 2,6-dimethyl-4-trifluoromethylpyridine-3-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,1,1-Trifluoro-2,4-pentanedione | HCID 73943 | — |
| Reactant | Methyl 3-aminocrotonate | HCID 643918 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | Methyl 2,6-dimethyl-4-trifluoromethylpyridine-3-carboxylate | HCID 23092426 | 71% |
Reaction Steps
1,1,1-Trifluoro-2,4-pentanedione (25.01 g, 135.3 mmol) was dissolved in acetonitrile (230 mL), followed by the addition of methyl 3-aminocrotonate (15.57 g, 135.2 mmol). The mixture was subjected to heating under reflux for 20 hours. The reaction mixture was allowed to cool down to room temperature, and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (silica gel: 400 g; developer: hexane:acetone=10:1) to obtain the title compound (22.30 g, 71%) as a yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07750150B2 |
| Source dataset | uspto-grants-2010_07 |
| ORD ID | ord-e0cb1b6b64084e03ab1d4297a603fa4c |
| Source note | uspto-grants-2010_07 |