1-Nitro-2,5-bis(trifluoromethyl)benzene → 2,5-Bis(trifluoromethyl)aniline

HRID 585334

反応式

HRID 585334 の反応式
[F:1][C:2]([F:17])([F:16])[C:3]1[CH:8]=[CH:7][C:6]([C:9]([F:12])([F:11])[F:10])=[CH:5][C:4]=1[N+:13]([O-])=O.[H][H]>[Ni].C(O)(C)C>[F:1][C:2]([F:16])([F:17])[C:3]1[CH:8]=[CH:7][C:6]([C:9]([F:10])([F:12])[F:11])=[CH:5][C:4]=1[NH2:13]

参加物

5

反応物 2

HCID 27340481-Nitro-2,5-bis(trifluoromethyl)benzeneHCID 178418361HCID 178418361、化合物

生成物 1

HCID 7198182,5-Bis(trifluoromethyl)aniline収率 73%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 3776Isopropanol溶媒

反応条件

温度
70 °C

実験手順

Into an autoclave, 1.05 g of Raney Nickel catalyst (10 wt %) and 100 ml of isopropanol were introduced, and 10.0 g of 2,5-bis(trifluoromethyl)nitrobenzene was added thereto in small amounts. Hydrogen gas was blown until 5 kg/cm2 with stirring, and the temperature was increased to 70° C. Reaction was carried out at from 70 to 90° C. for 8 hours. After the temperature was recovered to room temperature, hydrogen gas was evacuated, and the Raney Nickel was subjected to filtration and washed with isopropanol. The solvent was concentrated to obtain 2,5-bis(trifluoromethyl)aniline (6.42 g, yield 73%, purity by GC 99.4%). As a result of analysis by GC-Mass, 1H-NMR and 19F-NMR, the product was confirmed to be 2,5-bis(trifluoromethyl)aniline.

後処理

  1. customReaction
  2. customAfter the temperature was recovered to room temperature
  3. customhydrogen gas was evacuated
  4. filtrationthe Raney Nickel was subjected to filtration
  5. washwashed with isopropanol
  6. concentrationThe solvent was concentrated

出典と根拠

ORDレコード
ord-8eb358c7da34435c913e5460880d5ac0
出典データセット
uspto-grants-2005_08
特許番号
US06930214B2

関連ノート

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