反応 #1702063

ord-5882c151337f4c049761ccbd9576fef9

反応方程式

[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

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出extracted by ethyl acetate
  2. 2
    洗浄The organic layer was washed by water
  3. 3
    乾燥a saturated sodium hydrogen carbonate aq. solution, and a saturated saline solution, dried over magnesium sulfate
  4. 4
    濃縮concentrated under reduced pressure
  5. 5
    その他The crude product was purified by recrystallization in a solvent of hexane

実験手順

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%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08765719B2uspto-grants-2014_07