Реакция #691569

ord-cf88482514974e5585e925af2ec559e7

Уравнение реакции

C1CCNCC1
piperidine
O=C(CO)c1ccccc1
Hydroxyacetophenone
O=C([O-])[O-].[K+].[K+]
K2CO3
BrCc1ccccc1CBr
α,α′-dibromoxylol
CC(=O)c1ccc(OCc2ccc(CN3CCCCC3)cc2)cc1
α-(4-Acetylphenoxy)-α′-piperidino p-xylol

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураunder reflux
  2. 2
    ДругоеThe solvent was evaporated under reduced pressure
  3. 3
    Экстракцияextracted with methylene chloride
  4. 4
    ДругоеThe combined organic extracts were crystallized with oxalic acid
  5. 5
    ДругоеRecrystallization
  6. 6
    Другоеresulted in the pure product

Методика

Hydroxyacetophenone (2 mmol) and 5 mmol of K2CO3 were stirred in 20 ml of acetone with 2 ml of DMF for 10 minutes. After addition of 3.5 mmol of α,α′-dibromoxylol the reaction was stirred at ambient temperature for 12 hours and after addition of 7 mmol of piperidine for 1 hour under reflux. The solvent was evaporated under reduced pressure. The residue was suspended in water, extracted with methylene chloride. The combined organic extracts were crystallized with oxalic acid. Recrystallization resulted in the pure product.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07910605B2uspto-grants-2011_03