Chloroform → HCID 15614715, compound

HRID 893659Notes

Reaction equation

HRID 893659 reaction equation
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][NH:9][C:10]2[CH:11]=[N:12][CH:13]=[CH:14][C:15]=2[N+:16]([O-:18])=[O:17])=[CH:4][CH:3]=1.[Cl:19]C(Cl)Cl>>[ClH:19].[F:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:8][NH:9][C:10]2[CH:11]=[N:12][CH:13]=[CH:14][C:15]=2[N+:16]([O-:18])=[O:17])=[CH:6][CH:7]=1

Participants

3

Reactant 2

HCID 6212Chloroform2×HCID 156147143-(4-Fluorobenzylamino)-4-nitropyridine

Product 1

HCID 15614715HCID 15614715, compound

Procedure

To a stirred and cooled (0° C.) solution of 8.7 parts of N-[(4-fluorophenyl)methyl]-4-nitro-3-pyridinamine, 1-oxide and 150 parts of trichloromethane was added dropwise a solution of 10.2 parts of phosphor trichloride in 75 parts of trichloromethane. Upon completion, the mixture was allowed to reach room temperature and stirring was continued for one hour at reflux temperature. The reaction mixture was cooled and the solvent was evaporated. The residue was stirred intrichloromethane. The product was filtered off and dried, yielding 9 parts of N-[(4-fluorophenyl)methyl]-4-nitro-3-pyridinamine monohydrochloride (intermediate 13).

Workup

  1. customto reach room temperature
  2. stirringstirring
  3. temperatureat reflux temperature
  4. temperatureThe reaction mixture was cooled
  5. customthe solvent was evaporated
  6. stirringThe residue was stirred intrichloromethane
  7. filtrationThe product was filtered off
  8. customdried

Sources & evidence

ORD record
ord-0a7dfa2bfd6d49908c763fc7faac0a61
Source dataset
uspto-grants-1992_06
Patent number
US05126339

Reaction notes

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