反応 #417971

反応方程式

1,3-dibromo propane

cesium carbonate

DMF

2-chloro-5-nitro phenol

→

title compound 26a

2-(3-bromo-propoxy)-1-chloro-4-nitro benzene

溶媒

Water

反応条件

後処理

1. 1
   抽出extracted with DCM (3×25 mL)
2. 2
   乾燥were dried over sodium sulfate
3. 3
   濃縮concentrated in vacuo
4. 4
   その他The crude product was purified by flash column chromatography

実験手順

1,3-dibromo propane (1.3 mL, 12.65 mmol) and cesium carbonate (4.1 g, 12.65 mmol) was added to the DMF (18 mL) solution of 2-chloro-5-nitro phenol (2.0 g, 11.5 mmol) and the reaction mixture stirred overnight at room temperature. Water (20 mL) was added to the mixture, extracted with DCM (3×25 mL) and combined extracts were dried over sodium sulfate and concentrated in vacuo. The crude product was purified by flash column chromatography to get the title compound 26a in 64% (2.176 g) yield as colorless oil.

出典