HRID595612

反应详情

EQUATION

反应方程式

HRID 595612 的结构方程式

PROCEDURE

实验过程

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).

WORKUP

后处理

  1. customwas then tightly closed
  2. customto react at 170° C. for two hours
  3. temperatureThe product was then cooled
  4. customremoved from the autoclave
  5. additionThe product was diluted with toluene
  6. customthe resulting polyvinylbenzocyclobutene was precipitated in methanol
  7. filtrationPolyvinylbenzocyclobutene was filtered out
  8. customthe solvent was removed
  9. distillationThe residue was distilled under reduced pressure (127° C., 5 mmHg)