Реакция #84215

ord-c4265732d68d4518b7948f2f6db5f8ab

Растворители

Условия реакции

Температура
80°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураThe suspension was cooled to room temperature
  2. 2
    workup.STIRRINGunder stirring
  3. 3
    ТемператураThe heterogeneous mixture was cooled to 0 to 5° C. for 60 to 90 minutes
  4. 4
    Фильтрацияthe solid filtered on a gooch funnel
  5. 5
    Промывкаwashed with water (50 ml)
  6. 6
    ДругоеAn orange solid was obtained
  7. 7
    ДругоеIt was dried under vacuum at room temperature

Методика

3-hydroxy-4-(difluoromethoxy)-benzoic acid methyl ester (5 g, 22.9 mmol), K2CO3 (4.75 g, 34.4 mmol), NaI (0.34 g, 2.3 mmol) and bromo-methylcyclopropane (3.7 g, 27.5 mmol) were dissolved in DMF (25 ml), and the heterogeneous mixture was stirred and warmed at 80° C. for two hours. The suspension was cooled to room temperature, and water (50 ml) was added under stirring. The heterogeneous mixture was cooled to 0 to 5° C. for 60 to 90 minutes, and the solid filtered on a gooch funnel and washed with water (50 ml). An orange solid was obtained. It was dried under vacuum at room temperature. (yield 95.8%).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US09434691B2uspto-grants-2016_09