Methanol → 3,5,6-Trifluoropyridin-2-amine

HRID 1274663Notes

Reaction equation

HRID 1274663 reaction equation
CO.C([NH:10][C:11]1[C:16]([F:17])=[CH:15][C:14]([F:18])=[C:13]([F:19])[N:12]=1)C1C=CC=CC=1>[Pd].C(O)(=O)C>[NH2:10][C:11]1[C:16]([F:17])=[CH:15][C:14]([F:18])=[C:13]([F:19])[N:12]=1

Participants

5

Reactant 2

HCID 887MethanolHCID 22121263N-benzyl-3,5,6-trifluoropyridin-2-amine

Product 1

HCID 125080743,5,6-Trifluoropyridin-2-amineYield 81.5%

Reagents, catalysts & solvents 2

HCID 23938PalladiumCatalystHCID 176Acetic AcidSolvent

Procedure

To 40 ml of methanol were added 7.60 g of the crude 2-benzylamino-3,5,6-trifluoropyridine as described above together with 0.55 g of 10% palladium on carbon and 2 ml acetic acid, and the mixture was hydrogenated at 50° C. for one day. The catalyst was separated by filtration, and the solvent and the like were distilled off under reduced pressure. The precipitate was dispersed in n-hexane, and collected by filtration to obtain 3.85 g of the title compound as a colorless solid.

Workup

  1. customThe catalyst was separated by filtration
  2. distillationthe solvent and the like were distilled off under reduced pressure
  3. additionThe precipitate was dispersed in n-hexane
  4. filtrationcollected by filtration

Sources & evidence

ORD record
ord-2194eb4bd5e34f9f870485c35cd83f7f
Source dataset
uspto-grants-2000_12
Patent number
US06156903

Reaction notes

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