Reaktion #67724

Reaktionsgleichung

Sodium hydroxide

2,2-difluoro-benzo[1,3]dioxol-5-yl-acetonitrile

benzyltriethylammonium

chloride

1-bromo-2-chloroethane

→

1-(2,2-difluoro-benzo[1,3]dioxol-5-yl)-cyclopropanecarbonitrile

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionextracted with ethyl acetate
2. 2
   TrocknenThe combined organic layers were dried over sodium sulfate
3. 3
   Sonstigeevaporated to dryness

Vorschrift

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.

Quelle