Réaction #73556

ord-7ed85289fe0e4e46950710b1bf82c8b3

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

1-(2,2-Difluoro-benzo[1,3]dioxol-5-yl)-cyclopropanecarbonitrile 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. and 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: US08541453B2uspto-grants-2013_09