Ethanol → Ethyl 4-iodobenzoate
反応式
[I:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][CH:3]=1.S(Cl)(Cl)=O.[CH2:15](O)[CH3:16]>>[CH2:15]([O:7][C:6](=[O:8])[C:5]1[CH:9]=[CH:10][C:2]([I:1])=[CH:3][CH:4]=1)[CH3:16]参加物
4
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 an the residue kugelrohr distilled (100 degrees C.; 0.55 mm) to give the title compound as a colorless oil, PMR (CDCl3): δ 1.42 (3H, t, J~7 Hz), 4,4 (2H, q, J~7 Hz), 7.8 (4H).
後処理
- 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 an the residue kugelrohr
- distillationdistilled (100 degrees C.; 0.55 mm)
出典と根拠
- ORDレコード
- ord-788057af86b945868d94596518452f80
- 出典データセット
- uspto-grants-1993_09
- 特許番号
- US05248777
反応ノート
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