反应 #1318

反应方程式

4-iodobenzoic acid

ethanol

thionyl chloride

→

title compound

Ethyl-4-iodobenzoate

反应条件

后处理

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

实验过程

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).

来源