Sodium Iodide → Iodomethyl Benzoate
反応式
[C:1]([O:9][CH2:10]Cl)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[I-:12].[Na+]>C(#N)C.O>[C:1]([O:9][CH2:10][I:12])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1参加物
5
実験手順
Chloromethyl benzoate (2.87 g, 16.82 mmol) was dissolved in acetonitrile (20 mL) and treated portionwise with sodium iodide (5.04 g, 33.6 mmol). The resulting mixture was stirred at room temperature for 18 hours. The reaction mixture was diluted with water and extracted with ethyl acetate (×2). The ethyl acetate layers were combined, dried under magnesium sulfate and evaporated under reduced pressure. The residue was purified by column chromatography (Biotage SP4) eluting with a gradient of 0-20% ethyl acetate and iso-hexane. Product containing fractions were combined and evaporated under reduced pressure to give the title compound as a yellow oil (3.15 g);
後処理
- extractionextracted with ethyl acetate (×2)
- customdried under magnesium sulfate
- customevaporated under reduced pressure
- customThe residue was purified by column chromatography (Biotage SP4)
- washeluting with a gradient of 0-20% ethyl acetate and iso-hexane
- additionProduct containing fractions
- customevaporated under reduced pressure
出典と根拠
- ORDレコード
- ord-08f072f24cdd4520a94b8a11359c627c
- 出典データセット
- uspto-grants-2014_08
- 特許番号
- US08796283B2
反応ノート
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