反応 #67724

反応方程式

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

溶媒

water

反応条件

後処理

1. 1
   抽出extracted with ethyl acetate
2. 2
   乾燥The combined organic layers were dried over sodium sulfate
3. 3
   その他evaporated to dryness

実験手順

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.

出典