Hydrochloric Acid → Methyl 3-chloro-4-hydroxy-5-methoxybenzoate
反応式
[Cl:1][C:2]1[C:3]([OH:13])=[C:4]([O:11][CH3:12])[CH:5]=[C:6]([CH:10]=1)[C:7]([OH:9])=[O:8].Cl.[CH3:15]O>>[CH3:15][O:8][C:7](=[O:9])[C:6]1[CH:5]=[C:4]([O:11][CH3:12])[C:3]([OH:13])=[C:2]([Cl:1])[CH:10]=1参加物
4
実験手順
A mixture of 5-chlorovanillic acid (5.0 g, 24.6 mmol) and conc. HCl (5 ml) in MeOH (100 ml) is heated at reflux for 48 hours. The solvent is removed in vacuo and water is added to the residue to yield a white precipitate, which is collected by filtration, washed with water, and then dissolved in Et2O. The solution is dried (Na2SO4) and the solvent removed in vacuo to yield 3-Chloro-4-hydroxy-5-methoxy-benzoic acid methyl ester as a white solid.
後処理
- temperatureis heated
- temperatureat reflux for 48 hours
- customThe solvent is removed in vacuo and water
- additionis added to the residue
- customto yield a white precipitate, which
- filtrationis collected by filtration
- washwashed with water
- dissolutiondissolved in Et2O
- dry with materialThe solution is dried (Na2SO4)
- customthe solvent removed in vacuo
出典と根拠
- ORDレコード
- ord-2c8e8947864b433182c7571b797dd203
- 出典データセット
- uspto-grants-2015_09
- 特許番号
- US09139586B2
反応ノート
読み込み中…