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Hydrazine → 2,3,5,6-Tetrafluoro-4-hydrazinopyridine

HRID 2246171
Notes
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Reaction equation

HRID 2246171 reaction equation
[F:1][C:2]1[N:7]=[C:6]([F:8])[C:5]([F:9])=[C:4](F)[C:3]=1[F:11].[NH2:12][NH2:13]>ClCCl>[F:1][C:2]1[C:3]([F:11])=[C:4]([NH:12][NH2:13])[C:5]([F:9])=[C:6]([F:8])[N:7]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 9321HydrazineHCID 69690Pentafluoropyridine

Product 1

HCID 20640312,3,5,6-Tetrafluoro-4-hydrazinopyridine

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

Pentafluoropyridine (3.4 g; 20 mmol) was dissolved in dichloromethane (50 mL) and chilled in an ice bath. To the solution was added hydrazine (640 mg; 22 mmol) and it was stirred overnight. The solvent was evaporated, and the residue was dissolved in dichloromethane (50 mL) and washed with a 10% sodium carbonate solution (5 mL). It was dried over magnesium sulfate, and evaporated, to give crude 2,3,5,6-tetrafluoro-pyridin-4-yl-hydrazine. The crude product was then dissolved in ethanol. To the solution was added one drop of acetic acid, and m-tolylaldehyde (1.45 g; 12 mmol) and it was heated at 60° C. overnight. The resulting precipitate was filtered and dried to give N-(3-methyl-benzylidene)-N′-(2,3,5,6-tetrafluoro-pyridin-4-yl)-hydrazine (2.2 g).

Workup

  1. temperaturechilled in an ice bath
  2. customThe solvent was evaporated
  3. dissolutionthe residue was dissolved in dichloromethane (50 mL)
  4. washwashed with a 10% sodium carbonate solution (5 mL)
  5. dry with materialIt was dried over magnesium sulfate
  6. customevaporated

Sources & evidence

ORD record
ord-61c6e8d62aab413bbbb5cc9eb87ef1fc
Source dataset
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07687498B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes