Réaction #1702063

ord-5882c151337f4c049761ccbd9576fef9

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Extractionextracted by ethyl acetate
  2. 2
    LavageThe organic layer was washed by water
  3. 3
    Séchagea saturated sodium hydrogen carbonate aq. solution, and a saturated saline solution, dried over magnesium sulfate
  4. 4
    Concentrationconcentrated under reduced pressure
  5. 5
    AutreThe crude product was purified by recrystallization in a solvent of hexane

Mode opératoire

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%).

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US08765719B2uspto-grants-2014_07