2,3,4-Trifluoro-1-nitro-5-(trifluoromethyl)benzene → HCID 15614237, compound

HRID 1090863Notes

Reaction equation

HRID 1090863 reaction equation
[F:1][C:2]1[C:7]([F:8])=[C:6]([F:9])[C:5]([N+:10]([O-])=O)=[CH:4][C:3]=1[C:13]([F:16])([F:15])[F:14]>O1CCCC1.[Ni]>[F:1][C:2]1[C:7]([F:8])=[C:6]([F:9])[C:5]([NH2:10])=[CH:4][C:3]=1[C:13]([F:15])([F:16])[F:14]

Participants

4

Reactant 1

HCID 156142362,3,4-Trifluoro-1-nitro-5-(trifluoromethyl)benzene

Product 1

HCID 15614237HCID 15614237, compoundYield 87.9%

Reagents, catalysts & solvents 2

HCID 935NickelCatalystHCID 8028TetrahydrofuranSolvent

Procedure

35 g of 2,3,4-trifluoro-5-nitro-benzotrifluoride in 150 ml of tetrahydrofuran were initially introduced into a hydrogenation apparatus, 3 g of Raney nickel were added and, after flushing with nitrogen, the mixture was hydrogenated to constant pressure with 30 bar of hydrogen at 25° to 45° C. After completion of the hydrogen uptake, the pressure was released and the reaction solution was filtered and subsequently fractionally distilled. 27 g of 2,3,4-trifluoro-5-amino-benzotrifluoride were obtained with a boiling point of 82° to 83° C. at 15 mbar.

Workup

  1. additionwere added
  2. customafter flushing with nitrogen
  3. customwas hydrogenated to constant pressure with 30 bar of hydrogen at 25° to 45° C
  4. filtrationthe reaction solution was filtered
  5. distillationsubsequently fractionally distilled

Sources & evidence

ORD record
ord-2cdd080e605843298aca1d905ea8d5da
Source dataset
uspto-grants-1992_01
Patent number
US05082971

Reaction notes

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