Methanol → Methyl 4-Chloro-2-methylbenzoate
反応式
[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4]([CH3:11])[CH:3]=1.S(=O)(=O)(O)O.[OH-].[Na+].[CH3:19]O>>[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([O:8][CH3:19])=[O:7])=[C:4]([CH3:11])[CH:3]=1参加物
5
反応条件
- 温度
- 70 °C
実験手順
(Step 1) To a solution of 4-chloro-2-methylbenzoic acid (5.0 g) in methanol (40 ml) was added concentrated sulfuric acid at room temperature. The mixture was stirred at 70° C. for 3 hr, neutralized with 1N sodium hydroxide, and extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over magnesium sulfate, and filtered. The solvent was evaporated under reduced pressure. The residue was purified by silica gel chromatography (ethyl acetate:hexane=1:19→3:7) to give methyl 4-chloro-2-methylbenzoate (5.05 g) as an oil.
後処理
- extractionextracted with ethyl acetate
- washThe organic layer was washed with saturated brine
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- customThe solvent was evaporated under reduced pressure
- customThe residue was purified by silica gel chromatography (ethyl acetate:hexane=1:19→3:7)
出典と根拠
- ORDレコード
- ord-74550971c4074f288ddf333d0a5df061
- 出典データセット
- uspto-grants-2013_07
- 特許番号
- US08481569B2
反応ノート
読み込み中…