2-Bromo-6-chlorobenzoic acid → Methyl 2-bromo-6-chlorobenzoate
反応式
[Br:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([Cl:11])[C:3]=1[C:4]([OH:6])=[O:5].[CH3:12][Si](C=[N+]=[N-])(C)C>CO>[Br:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([Cl:11])[C:3]=1[C:4]([O:6][CH3:12])=[O:5]参加物
4
反応条件
- 温度
- 0 °C
実験手順
To a solution of 2-bromo-6-chlorobenzoic acid (17.7 g, 75.2 mmol) in methanol (200 mL) at 0° C. was added (trimethylsilyl)diazomethane (2M in hexanes, 100 mL, 0.200 mol). The solution was stirred at 0° C. for 1.5 hours, then warmed to room temperature and washed with aqueous sodium bicarbonate and brine, dried over Na2SO4, filtered and concentrated. The residue was subjected to silica gel chromatography eluted with 0-5% ethyl acetate in hexanes to provide methyl 2-bromo-6-chlorobenzoate as a pale yellow oil that gave proton NMR spectra consistent with theory.
後処理
- temperaturewarmed to room temperature
- washwashed with aqueous sodium bicarbonate and brine
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
- washeluted with 0-5% ethyl acetate in hexanes
出典と根拠
- ORDレコード
- ord-461a62a34e8f4c24b67ae45093547b47
- 出典データセット
- uspto-grants-2005_07
- 特許番号
- US06919343B2
反応ノート
読み込み中…