2-Cyano-3,5-difluoropyridine → HCID 58504005, compound

HRID 2407715Notes

Reaction equation

HRID 2407715 reaction equation
[F:1][C:2]1[C:3]([C:9]#[N:10])=[N:4][CH:5]=[C:6]([F:8])[CH:7]=1.[NH4+]=[S:12]>CO.O>[F:1][C:2]1[C:3]([C:9](=[S:12])[NH2:10])=[N:4][CH:5]=[C:6]([F:8])[CH:7]=1

Participants

4

Reactant 1

HCID 27832532-Cyano-3,5-difluoropyridine

Product 1

HCID 58504005HCID 58504005, compound

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 962WaterSolvent

Conditions

Temperature
0 °C

Procedure

3,5-Difluoropicolinonitrile (1.00 g) was partially dissolved in methanol (5 mL) and cooled to 0° C. A solution of ammonium sulfide in water (1.1 mL, 45% weight) was added slowly and the reaction was stirred 14 hours. The reaction was decanted and this solution was concentrated and then purified by column chromatography using dichloromethane as the eluant to obtain the title compound (0.17 g) having the following physical data.

Workup

  1. customThe reaction was decanted
  2. concentrationthis solution was concentrated
  3. custompurified by column chromatography

Sources & evidence

ORD record
ord-fea76909a9ec42f0b1aaeac3fd894a5e
Source dataset
uspto-grants-2014_08
Patent number
US08809538B2

Reaction notes

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