Реакция #2069931

ord-651364f736894c24b9436e1b8a8a9c0f

Растворители

Условия реакции

Температура
90°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Экстракцияextracted with toluene
  2. 2
    Промывкаthe toluene layer was well washed with water, and toluene
  3. 3
    Другоеwas evaporated away
  4. 4
    workup.ADDITION20 g of sodium hydroxide, 50 ml of water and 200 ml of ethanol were added to the resulting residue
  5. 5
    Температураrefluxed for 2 hours
  6. 6
    ДругоеEthanol was evaporated away
  7. 7
    workup.ADDITIONhydrochloric acid was added
  8. 8
    Экстракцияextracted with diethyl ether
  9. 9
    Сушкаdried with anhydrous magnesium sulfate
  10. 10
    ДругоеThe solvent was evaporated away
  11. 11
    Другоеthe resulting residue was recrystallized from a mixed solvent of ethanol and water

Методика

A solution comprising 14 g of allyl (4-chlorobutyl) ether, 14 g of 4-hydroxybenzoic acid, 14 g of potassium carbonate and 50 ml of dimethylformamide was stirred at 90° C. for 3 hours. Water was added to it, and extracted with toluene, and the toluene layer was well washed with water, and toluene was evaporated away. 20 g of sodium hydroxide, 50 ml of water and 200 ml of ethanol were added to the resulting residue, and refluxed for 2 hours. Ethanol was evaporated away, and hydrochloric acid was added to make it acidic, and then extracted with diethyl ether and dried with anhydrous magnesium sulfate. The solvent was evaporated away, and the resulting residue was recrystallized from a mixed solvent of ethanol and water to obtain 29 g of 4-(4-allyloxybutyloxy)benzoic acid.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07541071B2uspto-grants-2009_06