Sodium Iodide → Iodomethyl Benzoate
반응식
[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]=1참가 물질
5
실험 절차
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);
후처리
- 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
출처 및 근거
- ORD 기록
- ord-08f072f24cdd4520a94b8a11359c627c
- 출처 데이터셋
- uspto-grants-2014_08
- 특허 번호
- US08796283B2
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