반응식
[CH3:1][O:2][CH2:3][CH2:4][O:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([N+:12]([O-])=O)[C:7]=1[NH2:15].[OH-].[Na+]>C(OCC)(=O)C.C(O)C>[CH3:1][O:2][CH2:3][CH2:4][O:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([NH2:12])[C:7]=1[NH2:15]참가 물질
5
실험 절차
To a solution of 1 g 2-(2-Methoxy-ethoxy)-6-nitro-phenylamine in 10 mL ethyl acetate and 3 mL ethanol, 4.4 g SnCl2 dihydrate were added and the reaction mixture was heated to reflux for 6 h. Then, after cooling 50 mL 2 M NaOH were added and the inorganic precipitate was filtered and washed extensivley with ethyl acetate. The filtrate was extracted with exthyl acetate (3×100 ml), the combined organic layers were dried over MgSO4, and the solvents were removed under reduced pressure. The remaining product was pure enough for the next reaction step.
후처리
- temperaturethe reaction mixture was heated
- temperatureto reflux for 6 h
- additionwere added
- filtrationthe inorganic precipitate was filtered
- washwashed extensivley with ethyl acetate
- extractionThe filtrate was extracted with exthyl acetate (3×100 ml)
- dry with materialthe combined organic layers were dried over MgSO4
- customthe solvents were removed under reduced pressure
- customThe remaining product was pure enough for the next reaction step
출처 및 근거
- ORD 기록
- ord-7ca436af06dc497f9fc83b82dd2f06b1
- 출처 데이터셋
- uspto-grants-2010_06
- 특허 번호
- US07741341B2
연결된 노트
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