HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → methyl (E)-3-[4-(4-methylphenyl)thiophen-2-yl)acrylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 4-Methylphenyl borate | HCID 86645333 | — |
| Reactant | methyl (E)-3-(4-bromothiophen-2-yl)acrylic acid | HCID 86756172 | — |
| Catalyst | HCID 178418397 | HCID 178418397 | — |
| Solvent | Toluene-ethanol water | HCID 66602552 | — |
| Product | methyl (E)-3-[4-(4-methylphenyl)thiophen-2-yl)acrylate | HCID 86756171 | 76.5% |
Reaction Steps
Under argon atmosphere, a solution of methyl (E)-3-(4-bromothiophen-2-yl)acrylic acid (3.0 g), 4-methylphenyl borate (1.82 g) and potassium carbonate (3.36 g) in toluene-ethanol-water (120-12-12 ml) was stirred at room temperature for 1 hour. To the reaction mixture was added tetrakistriphenylphosphinepalladium (0.42 g), and the mixture was refluxed for 24 hours and cooled to room temperature. The organic layer was washed with saturated sodium chloride solution, dried with magnesium sulfate and concentrated under reduced pressure. The residue was separated and purified with column chromatography (ethyl acetate/hexane=1:9→1:5→1:2) to give methyl (E)-3-[4-(4-methylphenyl)thiophen-2-yl)acrylate (2.40 g) as pale yellow crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06166006 |
| Source dataset | uspto-grants-2000_12 |
| ORD ID | ord-e74206eea3ad4ae9a792fc6ab1e069de |
| Source note | uspto-grants-2000_12 |