Hydrochloric Acid → Methyl 5-Methoxy-2-methylbenzoate
反応式
Br[C:2]1[CH:3]=[C:4]([C:9]([O:11][CH3:12])=[O:10])[C:5]([CH3:8])=[CH:6][CH:7]=1.Cl.CN(C)[CH:16]=[O:17]>[Cu](I)I>[CH3:16][O:17][C:2]1[CH:3]=[C:4]([C:9]([O:11][CH3:12])=[O:10])[C:5]([CH3:8])=[CH:6][CH:7]=1参加物
5
実験手順
12.6 g of a 28% sodium methylate methanol solution and 4.2 g of copper iodide were added to 5 g of methyl 4-bromo-toluate dissolved in 20 ml of dimethylformamide and the mixture was refluxed under heating for 2 hours. The reaction mixture was adjusted to about pH 2 by adding 1N-hydrochloric acid thereto and extracted with ethyl acetate. and the organic layer was washed with a saturated saline solution and then dried over anhydrous sodium sulfate. The residue obtained by removing the solvent was applied to silica gel column chromatography to obtain 2.47 g of the title compound.
後処理
- temperaturethe mixture was refluxed
- temperatureunder heating for 2 hours
- extractionextracted with ethyl acetate
- washand the organic layer was washed with a saturated saline solution
- dry with materialdried over anhydrous sodium sulfate
- customThe residue obtained
- customby removing the solvent
出典と根拠
- ORDレコード
- ord-beabbc0321ac4c0eb03c5d181ea16308
- 出典データセット
- uspto-grants-1997_01
- 特許番号
- US05591752
反応ノート
読み込み中…