2,6-Dinitrophenol → 2-Amino-6-nitrophenol
反応式
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([N+:10]([O-])=O)[C:5]=1[OH:13])([O-:3])=[O:2]>C(OCC)(=O)C.[Pd]>[NH2:10][C:6]1[CH:7]=[CH:8][CH:9]=[C:4]([N+:1]([O-:3])=[O:2])[C:5]=1[OH:13]参加物
4
実験手順
A solution of 2,6-dinitrophenol (6.31 g, 27.4 mmol) in ethyl acetate (50 mL) was cooled to 0° C., 10% palladium activated carbon (250 mg) was added thereto, and the mixture was stirred under a hydrogen atmosphere for 5 hr. The reaction mixture was filtered through Celite (registered trademark) and the filtrate was concentrated under reduced pressure. The resulting residue was diluted with chloroform, anhydrous sodium sulfate was added thereto, and the mixture was stirred for 15 min. Anhydrous sodium sulfate was filtered off, followed by concentration under reduced pressure. The resulting residue was powdered with hexane and collected by filtration to afford 2-amino-6-nitrophenol as a brown amorphous substance (2.41 g).
後処理
- filtrationThe reaction mixture was filtered through Celite (registered trademark)
- concentrationthe filtrate was concentrated under reduced pressure
- additionThe resulting residue was diluted with chloroform, anhydrous sodium sulfate
- additionwas added
- stirringthe mixture was stirred for 15 min
- filtrationAnhydrous sodium sulfate was filtered off
- concentrationfollowed by concentration under reduced pressure
- filtrationcollected by filtration
出典と根拠
- ORDレコード
- ord-cdf280dc0212486fbf4705c1c538df93
- 出典データセット
- uspto-grants-2015_05
- 特許番号
- US09035059B2
反応ノート
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