Hydrochloric Acid → 3-Methyl-2-nitrobenzenemethanol
反応式
C[C:2]1[CH:3]=[CH:4][C:5]([N+:12]([O-:14])=[O:13])=[C:6]([CH:11]=1)[C:7]([O:9]C)=O.[BH4-].[Na+].[CH3:17]O.Cl>C1COCC1>[CH3:17][C:4]1[C:5]([N+:12]([O-:14])=[O:13])=[C:6]([CH:11]=[CH:2][CH:3]=1)[CH2:7][OH:9]参加物
6
実験手順
To a refluxed solution of methyl 5-methyl-2-nitrobenzoate (50 g, 0.256 mol) and sodium borohydride (29 g, 0.768 mol) in THF (400 mL) was added dropwise methanol (60 mL) over 2.5 h. After the addition was completed, the mixture was refluxed for 1 h and allowed to cool at room temperature. The excess reagent was decomposed by addition of diluted hydrochloric acid (300 mL) and the mixture was extracted with ethyl acetate. The organic layer was washed with brine, dried over magnesium sulfate, and concentrated to give 43.0 g of the title compound (100%).
後処理
- additionAfter the addition
- temperaturethe mixture was refluxed for 1 h
- extractionthe mixture was extracted with ethyl acetate
- washThe organic layer was washed with brine
- dry with materialdried over magnesium sulfate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-2edc453d54e8451783374ba4e7549129
- 出典データセット
- uspto-grants-1998_02
- 特許番号
- US05719152
反応ノート
読み込み中…