Methanol → Dimethyl 2-bromoterephthalate
反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[C:11]([O:13][CH3:14])=[O:12])[C:5]([OH:7])=[O:6].O=S(Cl)Cl.[CH3:19]O>>[Br:1][C:2]1[CH:3]=[C:4]([C:5]([O:7][CH3:19])=[O:6])[CH:8]=[CH:9][C:10]=1[C:11]([O:13][CH3:14])=[O:12]参加物
4
実験手順
To a solution of 3-bromo-4-(methoxycarbonyl)benzoic acid (3.0 g, 11.6 mmol) in MeOH (50 mL) was slowly added SOCl2 (2.76 g, 23.2 mmol) dropwise. After the addition completion, the reaction mixture was refluxed for 5 h. Then MeOH was removed and water was added. It was extracted with EA and the organic layer was washed with aqueous sodium bicarbonate solution, brine, dried over Na2SO4, filtered and concentrated under reduced pressure to give dimethyl 2-bromoterephthalate (3.1 g, yield 98%) as a white solid. It was used without further purification in the next step.
後処理
- temperatureAfter the addition completion, the reaction mixture was refluxed for 5 h
- customThen MeOH was removed
- additionwater was added
- extractionIt was extracted with EA
- washthe organic layer was washed with aqueous sodium bicarbonate solution, brine
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-2db9f10a59bb459a9d8a44d6b362e639
- 出典データセット
- uspto-grants-2013_10
- 特許番号
- US08546357B2
反応ノート
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