Реакция #51866

ord-603affca2e4842b7b2bec7915cb213f2

Реагенты

Нет

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Концентрированиеconcentrated sulfuric as a catalyst
  2. 2
    Другоеthe volatile fractions removed in vacuo
  3. 3
    workup.DISSOLUTIONThe residue was dissolved in ethyl ether (50 cm3)
  4. 4
    Промывкаwashed with water (25 cm3)
  5. 5
    Промывкаwashed with saturated sodium bicarbonate (25 cm3)
  6. 6
    Промывкаwashed with brine (25 cm3)
  7. 7
    Сушкаdried over magnesium sulfate, vacuum
  8. 8
    Фильтрацияfiltered
  9. 9
    Другоеthe filtrate volatile fractions removed in vacuo

Методика

To a solution of commercially available (3,4-dichloro-phenoxy)-acetic acid (2.65 g, 12.0 mmol) in allyl alcohol (12.0 cm3, 180 mmol) at ambient temperature under an atmosphere of dry nitrogen was added 4 drops concentrated sulfuric as a catalyst. The solution was stirred at ambient temperature for 20 hours and the volatile fractions removed in vacuo. The residue was dissolved in ethyl ether (50 cm3), washed with water (25 cm3), washed with saturated sodium bicarbonate (25 cm3), washed with brine (25 cm3), dried over magnesium sulfate, vacuum filtered and the filtrate volatile fractions removed in vacuo to afford the title compound as a colorless viscous oil (3.02 g, 96.8%) with positive ion ESI (M+H)+261.3.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US06852713B2uspto-grants-2005_02