Hydrochloric Acid → 6-Chloro-5-methoxynicotinic acid
반응식
C[O:2][C:3](=[O:13])[C:4]1[CH:9]=[C:8]([O:10][CH3:11])[C:7]([Cl:12])=[N:6][CH:5]=1.[OH-].[Na+].Cl>CO>[Cl:12][C:7]1[C:8]([O:10][CH3:11])=[CH:9][C:4]([C:3]([OH:13])=[O:2])=[CH:5][N:6]=1참가 물질
5
실험 절차
To a solution of 6-chloro-5-methoxynicotinic acid methyl ester (1.3 g, 6.4 mmol) in MeOH (4 mL) at 25° C. was added 10% NaOH aqueous solution (19.3 mmol). The reaction was stirred for 24 h, then placed into an ice water bath and acidified with 2M HCl until pH=2 was achieved. The flask was then placed into a refrigerator for 3 h. The white precipitate was filtered off and rinsed with cold H2O. The solid was dissolved in acetone, dried over MgSO4 and concentrated to furnish the product 6-chloro-5-methoxynicotinic acid as a yellow solid (0.895 g, 74%); 1H NMR (400 MHz, CDCl3) δ 8.45 (d, 1H), 7.66 (d, 1H), 3.83 (s, 3H).
후처리
- customplaced into an ice water bath
- waitThe flask was then placed into a refrigerator for 3 h
- filtrationThe white precipitate was filtered off
- washrinsed with cold H2O
- dissolutionThe solid was dissolved in acetone
- dry with materialdried over MgSO4
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-3e17597540444720aed008e94c68e7e4
- 출처 데이터셋
- uspto-grants-2012_05
- 특허 번호
- US08178565B2
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