HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,4,6-Trimethylpyridine → HCID 10194276, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,4,6-Trimethylpyridine | HCID 7953 | — |
| Reactant | 1,1,1-Trifluoro-4-(5-fluoro-2-methoxyphenyl)-4-methylpentan-2-one | HCID 10084920 | — |
| Reactant | HCID 178418306 | HCID 178418306 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 10194276 | HCID 10194276 | 30% |
Reaction Conditions
| Temperature | -70 °C |
|---|
Reaction Steps
tert-Butyl lithium (1.7 M in pentane, 0.5 mL) was added dropwise to a solution of 2,4,6-trimethylpyridine (0.12 g) in THF (0.5 mL) cooled to −70° C. under argon. The mixture was stirred at −70° C. for 15 minutes and 1,1,1-trifluoro-4-(5-fluoro-2-methoxyphenyl)-4-methylpentan-2-one (0.10 g) (Example 1) in THF (0.5 mL) was added. The reaction mixture was stirred for 20 minutes and then quenched with acetic acid. The mixture was diluted with EtOAc, washed with water, dried, filtered, and concentrated in vacuo. Fractionation by preparative layer chromatography on silica gel (methylene chloride-hexanes) followed by crystallization gave 43 mg of the title compound, m.p. 95° C.-98° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06903215B2 |
| Source dataset | uspto-grants-2005_06 |
| ORD ID | ord-5ad19718b1844c77af0e9a5b1024f650 |
| Source note | uspto-grants-2005_06 |