Chloroform → HCID 15614715, compound

HRID 1534720Notes

Reaction equation

HRID 1534720 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 1 hour at reflux temperature. The reaction mixture was cooled and the solvent was evaporated. The residue was stirred in trichloromethane. The product was filtered off and dried, yielding 9 parts of N-[(4-fluorophenyl)methyl]-4-nitro-3-pyridinamine monohydrochloride (intermediate 17).

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 in trichloromethane
  7. filtrationThe product was filtered off
  8. customdried

Sources & evidence

ORD record
ord-bdc5cb629a36407a90f432cf688a15a9
Source dataset
uspto-grants-1992_02
Patent number
USRE033833

Reaction notes

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