2,6-Dinitrophenol → 2-Amino-6-nitrophenol

HRID 576070ノート

反応式

HRID 576070 の反応式
[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

  1. filtrationThe reaction mixture was filtered through Celite (registered trademark)
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. additionThe resulting residue was diluted with chloroform, anhydrous sodium sulfate
  4. additionwas added
  5. stirringthe mixture was stirred for 15 min
  6. filtrationAnhydrous sodium sulfate was filtered off
  7. concentrationfollowed by concentration under reduced pressure
  8. 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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