HCID 51050006, compound → HCID 58336759, compound

HRID 2358979Notes

Reaction equation

HRID 2358979 reaction equation
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([N:7]2[CH:11]=[C:10]([C:12]3[N:17]=[C:16]([C:18]#[N:19])[CH:15]=[CH:14][CH:13]=3)[CH:9]=[N:8]2)[CH:2]=1.[NH4+]=[S:21]>N1C=CC=CC=1>[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([N:7]2[CH:11]=[C:10]([C:12]3[N:17]=[C:16]([C:18](=[S:21])[NH2:19])[CH:15]=[CH:14][CH:13]=3)[CH:9]=[N:8]2)[CH:2]=1

Participants

3

Reactant 1

HCID 51050006HCID 51050006, compound

Product 1

HCID 58336759HCID 58336759, compound

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Procedure

With heating, 1 g (4 mmol) of 6-(1-pyridin-3-yl-1H-pyrazol-4-yl)pyridine-2-carbonitrile was dissolved in 30 ml of pyridine, and 1.5 ml of ammonium sulphide (40% strength aqueous solution, corresponds to 8.8 mmol) were added. After 1 h, the mixture was concentrated by evaporation. The residue was recrystallized from ethanol with filtration of the hot mixture, the filtrate was concentrated slightly and the precipitate formed was filtered off with suction, washed with MTBE and dried on a rotary evaporator.

Workup

  1. temperatureWith heating
  2. concentrationthe mixture was concentrated by evaporation
  3. customThe residue was recrystallized from ethanol with filtration of the hot mixture
  4. concentrationthe filtrate was concentrated slightly
  5. customthe precipitate formed
  6. filtrationwas filtered off with suction
  7. washwashed with MTBE
  8. customdried on a rotary evaporator

Sources & evidence

ORD record
ord-59d44e3d33b64f9b965741f8a19b290c
Source dataset
uspto-grants-2014_04
Patent number
US08685964B2

Reaction notes

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