反応 #1318

反応方程式

4-iodobenzoic acid

ethanol

thionyl chloride

→

title compound

Ethyl-4-iodobenzoate

反応条件

後処理

1. 1
   温度the mixture was then heated
2. 2
   温度at reflux for 3 hours
3. 3
   その他Solvent was removed in vacuo
4. 4
   workup.DISSOLUTIONthe residue was dissolved in 100 ml ether
5. 5
   洗浄The ether solution was washed with saturated NaHCO3 and saturated NaCl solutions
6. 6
   乾燥dried (MgSO4)
7. 7
   その他Solvent was then removed in vacuo
8. 8
   workup.DISTILLATIONthe residue kugelrohr distilled (100 degrees C.; 0.55 mm)

実験手順

To a suspension of 10 g (40.32 mmol) of 4-iodobenzoic acid in 100 ml absolute ethanol was added 2 ml thionyl chloride and the mixture was then heated at reflux for 3 hours. Solvent was removed in vacuo and the residue was dissolved in 100 ml ether. The ether solution was washed with saturated NaHCO3 and saturated NaCl solutions and dried (MgSO4). Solvent was then removed in vacuo and the residue kugelrohr distilled (100 degrees C.; 0.55 mm) to give the title compound as a colorless oil, PMR (CDCl3): δ1.42 (3H, t, J~7 Hz), 4.4 (2H, q, J~7 Hz), 7.8 (4H).

出典