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

HRID 585334노트

반응식

HRID 585334 반응식
[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]

참가 물질

5

반응물 2

HCID 27340481-Nitro-2,5-bis(trifluoromethyl)benzeneHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 7198182,5-Bis(trifluoromethyl)aniline수율 73%

시약·촉매·용매 2

HCID 935Nickel촉매HCID 3776Isopropanol용매

반응 조건

온도
70 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8eb358c7da34435c913e5460880d5ac0
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06930214B2

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