Toluene → 1,2,3,4-Tetrahydro-1,1,4,4,6-pentamethylnaphthalene

HRID 266671

반응식

HRID 266671 반응식
Cl[C:2]([CH3:10])([CH2:4][CH2:5][C:6](Cl)([CH3:8])[CH3:7])[CH3:3].[Al+3].[Cl-].[Cl-].[Cl-].[C:15]1([CH3:21])[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1>>[CH3:21][C:15]1[CH:20]=[CH:19][C:18]2[C:6]([CH3:8])([CH3:7])[CH2:5][CH2:4][C:2]([CH3:10])([CH3:3])[C:17]=2[CH:16]=1

참가 물질

4

반응물 3

HCID 1140TolueneHCID 80360Hexane, 2,5-dichloro-2,5-dimethyl-HCID 6451240Aluminum(III) Chloride

생성물 1

HCID 811871,2,3,4-Tetrahydro-1,1,4,4,6-pentamethylnaphthalene수율 90%

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).

후처리

  1. additionadded portionwise to the solution
  2. extractionthe mixture was extracted with hexane
  3. washThe organic layer was washed each twice with water, aqueous sodium hydrogen carbonate
  4. dry with materialwith water, dried over MgSO4
  5. customthe solvent was removed by evaporation
  6. distillationThe residue was distilled

출처 및 근거

ORD 기록
ord-761b847cf8e74abd96bbc3c1bb21f911
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05652232

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