반응 #1318

반응 방정식

4-iodobenzoic acid

ethanol

thionyl chloride

→

title compound

Ethyl-4-iodobenzoate

반응 조건

후처리

1. 1
   온도the mixture was then heated
2. 2
   온도at reflux for 3 hours
3. 3
   기타Solvent was removed in vacuo
4. 4
   workup.DISSOLUTIONthe residue was dissolved in 100 ml ether
5. 5
   세척The ether solution was washed with saturated NaHCO3 and saturated NaCl solutions
6. 6
   건조dried (MgSO4)
7. 7
   기타Solvent was then removed in vacuo
8. 8
   workup.DISTILLATIONthe residue kugelrohr distilled (100 degrees C.; 0.55 mm)

실험 절차

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).

출처