반응 #353853

ord-761b847cf8e74abd96bbc3c1bb21f911

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONadded portionwise to the solution
  2. 2
    추출the mixture was extracted with hexane
  3. 3
    세척The organic layer was washed each twice with water, aqueous sodium hydrogen carbonate
  4. 4
    건조with water, dried over MgSO4
  5. 5
    기타the solvent was removed by evaporation
  6. 6
    workup.DISTILLATIONThe residue was distilled

실험 절차

2,5-Dichloro-2,5-dimethylhexane (67.5 g, 0.369 mol) was dissolved in dry toluene (200 ml), and then AlCl3 (4.05 g, 30.4 mmol) was crushed up and added portionwise to the solution. After being left for 2 hours, the reaction mixture was poured into ice/5% HCl and the mixture was extracted with hexane. The organic layer was washed each twice with water, aqueous sodium hydrogen carbonate, and then with water, dried over MgSO4, and the solvent was removed by evaporation. The residue was distilled to give 5,6,7,8-tetrahydro-2,5,5,8,8-pentamethylnaphthalene (70.42 g, yield: 90%). bp 100° C. (solidified at room temperature).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05652232uspto-grants-1997_07