HCID 20131629, compound → HCID 20131633, compound

HRID 845182Notes

Reaction equation

HRID 845182 reaction equation
[Cl:1][C:2]1[C:3]([O:11][C:12]2[C:17]([Cl:18])=[CH:16][CH:15]=[CH:14][C:13]=2[Cl:19])=[N:4][CH:5]=[C:6]([N+:8]([O-])=O)[CH:7]=1>C(O)(=O)C.O.[Fe]>[NH2:8][C:6]1[CH:7]=[C:2]([Cl:1])[C:3]([O:11][C:12]2[C:17]([Cl:18])=[CH:16][CH:15]=[CH:14][C:13]=2[Cl:19])=[N:4][CH:5]=1

Participants

5

Reactant 1

HCID 20131629HCID 20131629, compound

Product 1

HCID 20131633HCID 20131633, compound

Reagents, catalysts & solvents 3

HCID 23925IronCatalystHCID 176Acetic AcidSolventHCID 962WaterSolvent

Procedure

6.39 g (20 mmol) of 3-chloro-2-(2,6-dichlorophenoxy)-5nitropyridine were suspended in 7 ml of glacial acetic acid and 40 ml of water, and 5.6 g (0.1 mol) of iron powder were added in portions at room temperature (temperature 50° C.). The mixture was stirred for 1 hour, complete conversion determined by means of TLC, the mixture was filtered through a glass filter frit under suction, and the filter cake was carefully washed with ethyl acetate. The organic phase was washed with water until neutral, dried using MgSO4 and concentrated by evaporation.

Workup

  1. filtrationthe mixture was filtered through a glass
  2. filtrationfilter frit under suction
  3. washthe filter cake was carefully washed with ethyl acetate
  4. washThe organic phase was washed with water until neutral,
  5. customdried
  6. concentrationconcentrated by evaporation

Sources & evidence

ORD record
ord-1333dd1a02384ae09b6f704c7e9c3c73
Source dataset
uspto-grants-1988_07
Patent number
US04756739

Reaction notes

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