Реакция #2392212

ord-20f2ed60c5624ca9abb87e6c111d4b0e

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.ADDITIONwas slowly added dropwise
  2. 2
    workup.ADDITIONAfter completion of the addition
  3. 3
    workup.STIRRINGthe reaction mixture was further stirred at room temperature for 30 minutes
  4. 4
    Экстракцияextracted twice with diethyl ether
  5. 5
    Промывкаwashed with water
  6. 6
    Сушкаdried over anhydrous magnesium sulfate
  7. 7
    Концентрированиеconcentrated
  8. 8
    Другоеto give a crude product

Методика

First, 0.45 g of 5-(2,6-dichloro-4-(3,3-dichloro-2-propenyloxy)phenoxy)pentyloxyacetone oxime, 0.12 g of triethylamine, and 10 ml of tetrahydrofuran were placed in a reaction vessel, to which 0.25 g of 4-trifluoromethylbenzoyl chloride was slowly added dropwise with stirring at room temperature. After completion of the addition, the reaction mixture was further stirred at room temperature for 30 minutes, poured into diluted hydrochloric acid, and extracted twice with diethyl ether. The diethyl ether layers were combined, washed with water, dried over anhydrous magnesium sulfate, and concentrated to give a crude product. This crude product was subjected to silica gel chromatography, which afforded 0.59 g (yield, 96%) of 5-(2,6-dichloro-4-(3,3-dichloro-2-propenyloxy)phenoxy)pentyloxyacetone O-(4-trifluoromethylbenzoyl)oxime, nD25.6 1.5300.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US06437184B1uspto-grants-2002_08