HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tetrahydrofuran → HCID 86583978, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Ethyl 2-butynoate | HCID 78043 | — |
| Reactant | Tris(2,6-dimethoxyphenyl)phosphine | HCID 2734597 | — |
| Reactant | HCID 87842257 | HCID 87842257 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Product | HCID 86583978 | HCID 86583978 | — |
Reaction Steps
To a solution of 1,3-dichloro-phenyl acetylene (6.07 g, 35.5 mmol) in dry THF (60 mL) was added palladium acetate (186 mg, 0.68 mmol), ethyl 2-butynoate (5.97 g, 53.2 mmol) and tris (2,6-dimethoxyphenyl)phosphine (316 mg, 0.68 mmol) at room temperature. The reaction mixture was stirred for 18 h and filtered. The filtrate was washed with water (10 mL), and the water phase was extracted with ether (10 mL). The combined organic phases were dried and evaporated. The residue was purified by column chromatography using heptane:THF (20:1) as eluent. (E)-3-Methyl-5-(3,5-dichloro-phenyl)-pent-2-en-4-ynoic acid ethyl ester was isolated in 4.65 g (46%) yield.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06569901B2 |
| Source dataset | uspto-grants-2003_05 |
| ORD ID | ord-126689e2f1ed42579ce4619070a7149b |
| Source note | uspto-grants-2003_05 |