Réaction #67724

ord-b5f7da59d0044b58b7f926938dd088e6

Solvants

Conditions de réaction

Température
70°CELSIUS
Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Extractionextracted with ethyl acetate
  2. 2
    SéchageThe combined organic layers were dried over sodium sulfate
  3. 3
    Autreevaporated to dryness

Mode opératoire

Sodium hydroxide (50% aqueous solution, 10 mL) was slowly added to a mixture of crude (2,2-difluoro-benzo[1,3]dioxol-5-yl-acetonitrile, benzyltriethylammonium, chloride (3.00 g, 15.3 mmol), and 1-bromo-2-chloroethane (4.9 g, 38 mmol) at 70° C. The mixture was stirred overnight at 70° C. before the reaction mixture was diluted with water (30 mL) and extracted with ethyl acetate. The combined organic layers were dried over sodium sulfate and evaporated to dryness to give crude 1-(2,2-difluoro-benzo[1,3]dioxol-5-yl)-cyclopropanecarbonitrile, which was used directly in the next step.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US08524910B2uspto-grants-2013_09