Silicon carbide → 2,4,5-Trimethoxyaniline
反応式
[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]参加物
5
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-4a9620286f364daf8a781c1aa480f17a
- 出典データセット
- uspto-grants-1987_12
- 特許番号
- US04714700
反応ノート
読み込み中…