Methanol → Methyl 3-chloro-2-methylbenzoate
反応式
[Cl:1][C:2]1[C:3]([CH3:11])=[C:4]([CH:8]=[CH:9][CH:10]=1)[C:5]([OH:7])=[O:6].[CH3:12]O>S(=O)(=O)(O)O>[Cl:1][C:2]1[C:3]([CH3:11])=[C:4]([CH:8]=[CH:9][CH:10]=1)[C:5]([O:7][CH3:12])=[O:6]参加物
4
実験手順
To a solution of 3-chloro-2-methylbenzoic acid (1.00 g, 5.86 mmol) in methanol (25 mL) was added 3 drops of sulfuric acid. The mixture was stirred at reflux for 18 h. After concentrating the residue was dissolved in ether, washed with 10% sodium hydroxide solution, brine and dried (Na2SO4). Removal of the solvent under reduced pressure gave 0.95 g (88%) of the title compound as a white solid: 1H NMR (250 MHz, CDCl3) d 7.62 (d, 1H), 7.41 (d, 1H), 7.05 (t, 1H), 3.82 (s, 3H), 2.55 (s, 3H).
後処理
- temperatureat reflux for 18 h
- concentrationAfter concentrating the residue
- dissolutionwas dissolved in ether
- washwashed with 10% sodium hydroxide solution, brine
- dry with materialdried (Na2SO4)
- customRemoval of the solvent under reduced pressure
出典と根拠
- ORDレコード
- ord-a046e69c443c4c6d8b7aa4b22e57f729
- 出典データセット
- uspto-grants-2002_03
- 特許番号
- US06353116B1
反応ノート
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