1-Propanol → HCID 21102306, compound

HRID 1353116Notes

Reaction equation

HRID 1353116 reaction equation
[Cl:1][C:2]1[C:3](F)=[N:4][C:5]([F:9])=[C:6]([F:8])[CH:7]=1.O.[NH2:12][NH2:13].C(O)CC>ClC>[Cl:1][C:2]1[C:3]([NH:12][NH2:13])=[N:4][C:5]([F:9])=[C:6]([F:8])[CH:7]=1

Participants

5

Reactant 3

HCID 10311-PropanolHCID 24654Hydrazine hydrate (1:1)HCID 27832523-Chloro-2,5,6-trifluoropyridine

Product 1

HCID 21102306HCID 21102306, compoundYield 85.24%

Reagents, catalysts & solvents 1

HCID 6327Methyl ChlorideSolvent

Procedure

16.6 g of the compound obtained in Step 1 and 20.12 ml of hydrazine monohydrate were added to 100 ml of n-propanol, and the resulting mixture was refluxed 3 hours, and distilled under a reduced pressure to remove the solvent. The residue thus obtained was dissolved in 100 ml of chloromethane, washed with water, and dried over anhydrous magnesium sulfate. The dried organic layer was concentrated under a reduced pressure to obtain 15.9 g (yield: 85.24%) of the title compound.

Workup

  1. temperaturethe resulting mixture was refluxed 3 hours
  2. distillationdistilled under a reduced pressure
  3. customto remove the solvent
  4. customThe residue thus obtained
  5. washwashed with water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationThe dried organic layer was concentrated under a reduced pressure

Sources & evidence

ORD record
ord-34b17cc28e6745c6a92c05a75ed6c6d8
Source dataset
uspto-grants-2007_05
Patent number
US07220863B2

Reaction notes

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