Potassium Iodide → Methyl 4-(2-iodoethyl)benzoate
反応式
Cl[CH2:2][CH2:3][C:4]1[CH:13]=[CH:12][C:7]([C:8]([O:10][CH3:11])=[O:9])=[CH:6][CH:5]=1.[I-:14].[K+]>C(#N)C>[I:14][CH2:2][CH2:3][C:4]1[CH:13]=[CH:12][C:7]([C:8]([O:10][CH3:11])=[O:9])=[CH:6][CH:5]=1参加物
4
実験手順
70 g (352.4 mmol) of methyl 4-(2-chloroethyl)benzoate [CAS Reg. No. 65787-72-6] and 146.2 g (880.9 mmol) of potassium iodide are suspended in 800 ml of acetonitrile and stirred under reflux for three days. After the reaction has gone to completion, the reaction solution is cooled and filtered, and the filtrate is evaporated to dryness under reduced pressure. The resulting residue is purified by flash chromatography on silica gel (mobile phase: petroleum ether/ethyl acetate 30:1→20:1). This gives 101 g (348.3 mmol, 98.8% of theory) of a yellowish oil.
後処理
- temperatureunder reflux for three days
- temperaturethe reaction solution is cooled
- filtrationfiltered
- customthe filtrate is evaporated to dryness under reduced pressure
- customThe resulting residue is purified by flash chromatography on silica gel (mobile phase: petroleum ether/ethyl acetate 30:1→20:1)
出典と根拠
- ORDレコード
- ord-73622908ca18476080d1858fe349cd55
- 出典データセット
- uspto-grants-2012_07
- 特許番号
- US08217063B2
反応ノート
読み込み中…