Silicon carbide → 2,4,5-Trimethoxyaniline
반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[C:6]([O:11][CH3:12])=[CH:5][C:4]=1[N+:13]([O-])=O.[C-]#[Si+].[OH-].[Na+]>Cl>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[C:6]([O:11][CH3:12])=[CH:5][C:4]=1[NH2:13]참가 물질
5
실험 절차
Into a 500 cm3 flask, provided with a cooling device, were added successively 21.3 g (0.1 mole) of 2,4,5-trimethoxy nitrobenzene, 80 g of chemically pure stannous chloride for mirror making, 100 cm3 of a hydrochloric acid solution (d=1.18) and carborundum. The mixture was brought to boiling under reflux for 1 h. After cooling, a caustic soda solution was added until the precipitate disolved. The solution obtained was extracted with methylene chloride. The organic extracts were dried over sodium sulfate then evaporated under reduced pressure. The residue obtained was crystallized in ethanol.
후처리
- customInto a 500 cm3 flask, provided with a cooling device
- temperatureunder reflux for 1 h
- temperatureAfter cooling
- customThe solution obtained
- extractionwas extracted with methylene chloride
- dry with materialThe organic extracts were dried over sodium sulfate
- customthen evaporated under reduced pressure
- customThe residue obtained
- customwas crystallized in ethanol
출처 및 근거
- ORD 기록
- ord-4a9620286f364daf8a781c1aa480f17a
- 출처 데이터셋
- uspto-grants-1987_12
- 특허 번호
- US04714700
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