Hydrochloric Acid → 3-Cyano-4-methoxybenzoic acid
反応式
[C:1]([C:3]1[CH:4]=[C:5]([CH:10]=[CH:11][C:12]=1[O:13][CH3:14])[C:6]([O:8]C)=[O:7])#[N:2].CO.[Li+].[OH-].Cl>C1COCC1.O>[C:1]([C:3]1[CH:4]=[C:5]([CH:10]=[CH:11][C:12]=1[O:13][CH3:14])[C:6]([OH:8])=[O:7])#[N:2]参加物
7
実験手順
To a stirred solution of methyl 3-cyano-4-methoxybenzoate (1.1 g, 5.70 mmol) in a mixture of THF (70 mL), MeOH (70 mL) and water (5 mL) was added LiOH (0.97 g, 23.01 mmol) at RT and the reaction mixture was then stirred at RT for 1 h. The reaction mixture was acidified to pH ˜2 with 2 N HCl and the aqueous layer was extracted with DCM (3×100 mL). The combined organic extracts were washed with water (50 mL) and brine (50 mL), dried over anhydrous Na2SO4, filtered and evaporated under reduced pressure to afford 3-cyano-4-methoxybenzoic acid (1.0 g, 100%) as a solid.
後処理
- extractionthe aqueous layer was extracted with DCM (3×100 mL)
- washThe combined organic extracts were washed with water (50 mL) and brine (50 mL)
- dry with materialdried over anhydrous Na2SO4
- filtrationfiltered
- customevaporated under reduced pressure
出典と根拠
- ORDレコード
- ord-90cbbc102db3407ca3026f0cad53c7bf
- 出典データセット
- uspto-grants-2011_12
- 特許番号
- US08071595B2
反応ノート
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