HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic acid, 2-(triphenylphosphoranylidene)-, ethyl ester → (E)-Ethyl 3-(3-Chlorobicyclo[2.2.1]hept-2-en-2-yl)acrylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic acid, 2-(triphenylphosphoranylidene)-, ethyl ester | HCID 70670 | — |
| Reactant | 3-Chlorobicyclo[2.2.1]hept-2-ene-2-carbaldehyde | HCID 58044011 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | (E)-Ethyl 3-(3-Chlorobicyclo[2.2.1]hept-2-en-2-yl)acrylate | HCID 58043644 | 46% |
Reaction Steps
To a solution of 167a (9.0 g, 57.7 mmol) in methylene chloride (250 mL) was added ethyl 2-(triphenyl-λ5-phosphanylidene)acetate (20 g, 57.7 mmol). The mixture was stirred at room temperature overnight. It was then evaporated under reduced pressure. The residue was purified by silica-gel column chromatography eluting with 1:100 ethyl acetate/petroleum ether to afford 167b as a yellow oil (6.0 g, 46%). MS: [M+H]+ 227.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09238655B2 |
| Source dataset | uspto-grants-2016_01 |
| ORD ID | ord-82aa937b53f44a08a6f946849190585b |
| Source note | uspto-grants-2016_01 |