関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dicyclopentadiene | HCID 6492 | — |
| 反応物 | 4-tert-Butylcatechol | HCID 7381 | — |
| 反応物 | 2-Ethenylbicyclo[4.2.0]octa-1,3,5-triene | HCID 71341282 | — |
| 生成物 | 5-(4-Benzocyclobutenyl)-2-norbornene | HCID 86722209 | 42.9% |
反応手順
A 100-ml autoclave with an agitator was charge with 10 g (77 mmol) of 4-vinylbenzocyclobutene, 4.6 g (35 mmol) of dicyclopentadiene, and 438 mg (2.6 mmol) of 4-tert-butylcatechol and was then tightly closed. The reactants were allowed to react at 170° C. for two hours while stirring at 300 rpm. The product was then cooled and removed from the autoclave. The product was diluted with toluene, and the resulting polyvinylbenzocyclobutene was precipitated in methanol. Polyvinylbenzocyclobutene was filtered out, and the solvent was removed. The residue was transferred to a distillation apparatus. The residue was distilled under reduced pressure (127° C., 5 mmHg) to yield 3.0 g (15 mmol, yield 20%) of 5-(4-benzocyclobutenyl)-2-norbornene as a colorless and transparent liquid. 1H NMR structural identification showed that the present example produced a compound having the formula (2).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09243098B2 |
|---|
| 出典データセット | uspto-grants-2016_01 |
|---|
| ORD ID | ord-c58c343648814098baf3e3341b3c4320 |
|---|
| 出典メモ | uspto-grants-2016_01 |
|---|