Реакция #1702063

ord-5882c151337f4c049761ccbd9576fef9

Уравнение реакции

[Al+3].[Cl-].[Cl-].[Cl-]
AlCl3
[Al+3].[Cl-].[Cl-].[Cl-]
aluminum chloride
Oc1ccccc1
phenol
ClCCl
dichloromethane
[Al+3].[Cl-].[Cl-].[Cl-]
aluminum chloride
CC(C)(Cl)CCC(C)(C)Cl
2,5-dichloro-2,5-dimethylhexane
CC1(C)CCC(C)(C)c2cc(O)ccc21
5,6,7,8-tetrahydro-2-hydroxy-5,5,8,8-tetramethyl naphthalene

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Экстракцияextracted by ethyl acetate
  2. 2
    ПромывкаThe organic layer was washed by water
  3. 3
    Сушкаa saturated sodium hydrogen carbonate aq. solution, and a saturated saline solution, dried over magnesium sulfate
  4. 4
    Концентрированиеconcentrated under reduced pressure
  5. 5
    ДругоеThe crude product was purified by recrystallization in a solvent of hexane

Методика

The synthesis process is as set forth in the chemical reaction formula below. The AlCl3 in the reaction path stands for aluminum chloride. Into phenol (1.02 g, 10.8 mmol) were added anhydrous dichloromethane (5 mL), aluminum chloride (144 mg, 1.08 mmol), and 2,5-dichloro-2,5-dimethylhexane (2.18 g, 11.9 mmol) followed by stirring at room temperature for 19 hours. The reaction solution was poured into cold water and extracted by ethyl acetate. The organic layer was washed by water, a saturated sodium hydrogen carbonate aq. solution, and a saturated saline solution, dried over magnesium sulfate, and concentrated under reduced pressure. The crude product was purified by recrystallization in a solvent of hexane. The yield was 1.83 g (83%).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08765719B2uspto-grants-2014_07