HRID1222
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
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).
WORKUP
后处理
- temperaturethe mixture was then heated
- temperatureat reflux for 3 hours
- customSolvent was removed in vacuo
- dissolutionthe residue was dissolved in 100 ml ether
- washThe ether solution was washed with saturated NaHCO3 and saturated NaCl solutions
- dry with materialdried (MgSO4)
- customSolvent was then removed in vacuo
- distillationthe residue kugelrohr distilled (100 degrees C.; 0.55 mm)