反応 #66019

反応方程式

sulphonic acid

4-(4-fluorophenoxy)benzenesulphonic acid

thionyl chloride

→

4-(4-Fluoro-phenoxy)-benzenesulphonyl chloride

溶媒

DMF

反応条件

後処理

1. 1
   温度at reflux
2. 2
   その他The solvent was evaporated
3. 3
   workup.DISSOLUTIONthe residue dissolved in Et2O (40 mL)
4. 4
   洗浄The ether solution was washed with 5% aqueous NaOH (3×40 mL) and water (6×40 mL)
5. 5
   乾燥dried over anhydrous MgSO4
6. 6
   ろ過filtered
7. 7
   濃縮concentrated in vacuo
8. 8
   その他After drying in high vacuum overnight
9. 9
   その他the pure product was obtained as a white solid

実験手順

The sulphonic acid intermediate (2b) was then dissolved in an excess of thionyl chloride, a catalytic amount of DMF (few drops) was added, and the resulting mixture was stirred for 6 h at reflux. The solvent was evaporated and the residue dissolved in Et2O (40 mL). The ether solution was washed with 5% aqueous NaOH (3×40 mL) and water (6×40 mL), dried over anhydrous MgSO4, filtered, and concentrated in vacuo. After drying in high vacuum overnight, the pure product was obtained as a white solid. Yield: 1.04 g, 3.63 mmol, 72% (white solid). 1H-NMR (CDCl3): δ 7.99 (d, 3J=9.1 Hz, 2H, ArH), 7.19-7.02 (m, 6H, ArH).

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