反応 #1976199

反応方程式

1,2-difluoro-3-methylbenzene

bromine

→

1-Bromo-3,4-difluoro-2-methylbenzene

反応条件

後処理

1. 1
   温度dropwise maintaining a temperature of <30° C. with ice cooling
2. 2
   その他The mixture was partitioned between water (50 mL) and diethyl ether (100 mL)
3. 3
   抽出The aqueous phase was extracted with diethyl ether (3×50 mL)
4. 4
   洗浄were washed with water (50 mL), 5% sodium thiosulfate solution (50 mL), water (50 mL), brine (50 mL)
5. 5
   乾燥dried over anhydrous magnesium sulfate
6. 6
   濃縮concentrated in vacuo
7. 7
   その他to afford product in 8.07 g
8. 8
   その他(Caution: by of product=68-70° C. @ 57 mBar)

実験手順

To 1,2-difluoro-3-methylbenzene (5 g, 39.0 mmol, commercially available from e.g. Sigma-Aldrich, Apollo or Fluorochem) containing iron (0.131 g, 2.342 mmol) was added bromine (2.011 ml, 39.0 mmol) dropwise maintaining a temperature of <30° C. with ice cooling. The mixture was stirred at room temperature overnight. The mixture was partitioned between water (50 mL) and diethyl ether (100 mL). The aqueous phase was extracted with diethyl ether (3×50 mL), combined organic extracts were washed with water (50 mL), 5% sodium thiosulfate solution (50 mL), water (50 mL), brine (50 mL), dried over anhydrous magnesium sulfate and concentrated in vacuo to afford product in 8.07 g. (Caution: by of product=68-70° C. @ 57 mBar).

出典