Реакция #53569

ord-dc0f6da8f3b045d2a4076930466059c1

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеThe resulting reaction mixture
  2. 2
    Экстракцияthe organic matters were extracted with 20 ml of ethyl acetate twice
  3. 3
    Промывкаwashed with 30 ml of water twice
  4. 4
    Сушкаdried over anhydrous magnesium sulfate
  5. 5
    workup.DISTILLATIONthe ethyl acetate was distilled off under reduced pressure
  6. 6
    ДругоеPurification of the residue by thin layer chromatography

Методика

1.52 g (5.0 nmol) of methyl 2-chloro-4-(3-trifluoromethylpyrazolyl)benzoate, 0.66 g (8.6 mmol) of 1-propanethiol and 0.83 g (6.0 mmol) of potassium carbonate were stirred in 5 ml of N,N-dimethylformamide at 60° C. for 24 hours. The resulting reaction mixture was poured into 50 ml of water, and the organic matters were extracted with 20 ml of ethyl acetate twice. The ethyl acetate layers were combined, washed with 30 ml of water twice and dried over anhydrous magnesium sulfate, and the ethyl acetate was distilled off under reduced pressure. Purification of the residue by thin layer chromatography afforded 0.31 g of methyl 2-propylthio-4-(3-trifluoromethylpyrazolyl)benzoate as a white powder (m.p. 114-116° C.).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US06858639B2uspto-grants-2005_02