Methanol → Methyl 2-chloro-5-methoxy-4-nitrobenzoate
반응식
[Cl:1][C:2]1[CH:10]=[C:9]([N+:11]([O-:13])=[O:12])[C:8]([O:14][CH3:15])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].S(=O)(=O)(O)O.[CH3:21]O>>[Cl:1][C:2]1[CH:10]=[C:9]([N+:11]([O-:13])=[O:12])[C:8]([O:14][CH3:15])=[CH:7][C:3]=1[C:4]([O:6][CH3:21])=[O:5]참가 물질
4
실험 절차
A solution of 2-chloro-5-methoxy-4-nitrobenzoic acid (1 mmol) and concentrated sulfuric acid (0.02 mmol) in methanol (200 mL) was heated to reflux for 42 hours. The solvents were evaporated under reduced pressure then the residue partitioned between EtOAc (25 mL) and water (25 mL). The separated aqueous phase was extracted with EtOAc (3×25 mL), then the combined organic extracts were dried (Na2SO4) and concentrated under reduced pressure to afford the title compound (71%) as a solid.
후처리
- temperatureto reflux for 42 hours
- customThe solvents were evaporated under reduced pressure
- customthe residue partitioned between EtOAc (25 mL) and water (25 mL)
- extractionThe separated aqueous phase was extracted with EtOAc (3×25 mL)
- dry with materialthe combined organic extracts were dried (Na2SO4)
- concentrationconcentrated under reduced pressure
출처 및 근거
- ORD 기록
- ord-e3c0aea2e8f442948cbd6ab9ff921168
- 출처 데이터셋
- uspto-grants-2014_05
- 특허 번호
- US08716287B2
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