Methyl 5-methoxy-2-nitrobenzoate → 5-Methoxy-2-nitrobenzoic acid
반응식
C[O:2][C:3](=[O:15])[C:4]1[CH:9]=[C:8]([O:10][CH3:11])[CH:7]=[CH:6][C:5]=1[N+:12]([O-:14])=[O:13]>C(O)C.[OH-].[Na+]>[CH3:11][O:10][C:8]1[CH:7]=[CH:6][C:5]([N+:12]([O-:14])=[O:13])=[C:4]([CH:9]=1)[C:3]([OH:15])=[O:2]참가 물질
4
실험 절차
The crude material from Example 44b (23.3 g) is dissolved in 110 ml ethanol and 44 ml of 4N NaOH. The mixture is stirred at rt for 18 h. After that time, the ethanol is evaporated. To the residue, water is added and the mixture is washed twice with dichloromethane. To the water phase, conc. HCl is added until pH=1 is reached. The title compound is obtained by extraction with ether. Purification follows by crystallization from ethyl acetate-hexane. mp: 131-134° C.; MS: 196 (M+−1); HPLC: tret=7.90 min (Grad 1).
후처리
- customAfter that time, the ethanol is evaporated
- additionTo the residue, water is added
- washthe mixture is washed twice with dichloromethane
- additionTo the water phase, conc. HCl is added until pH=1
출처 및 근거
- ORD 기록
- ord-d4fc026c49264179b6c8cb3a7f6c1101
- 출처 데이터셋
- uspto-grants-2011_08
- 특허 번호
- US07998972B2
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