Hydrochloric Acid → 3-Cyano-4-methoxybenzoic acid
반응식
[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]참가 물질
7
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-90cbbc102db3407ca3026f0cad53c7bf
- 출처 데이터셋
- uspto-grants-2011_12
- 특허 번호
- US08071595B2
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