Potassium thiocyanate → (3-Chloro-2-methylphenyl)thiosemicarbazide

HRID 1654068Notes

Reaction equation

HRID 1654068 reaction equation
Cl.[Cl:2][C:3]1[C:4]([CH3:11])=[C:5]([NH:9][NH2:10])[CH:6]=[CH:7][CH:8]=1.[S-:12][C:13]#[N:14].[K+]>C(O)C>[Cl:2][C:3]1[C:4]([CH3:11])=[C:5]([NH:9][NH:10][C:13]([NH2:14])=[S:12])[CH:6]=[CH:7][CH:8]=1

Participants

4

Reactant 2

HCID 516872Potassium thiocyanateHCID 12732296(3-Chloro-2-methylphenyl)hydrazine hydrochloride

Product 1

HCID 20079518(3-Chloro-2-methylphenyl)thiosemicarbazide

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

19.3 g (0.1 mole) of 3-chloro-2-methylphenylhydrazinehydrochloride were dissolved in 200 ml of absolute ethanol. 11.64 g (0.12 mole) of potassium thiocyanate were added to the solution, and the mixture was heated during reflux for 16 hours. The mixture was then cooled, whereby the product was partially precipitated, and the mixture was subsequently evaporated to dryness by means of a rotating evaporator. The product was recrystallized from 200 ml water and 250 ml methanol, separated by filtration and washed thoroughly with water.

Workup

  1. temperaturethe mixture was heated
  2. temperatureduring reflux for 16 hours
  3. temperatureThe mixture was then cooled
  4. customwhereby the product was partially precipitated
  5. customthe mixture was subsequently evaporated to dryness by means of a rotating evaporator
  6. customThe product was recrystallized from 200 ml water and 250 ml methanol
  7. customseparated by filtration
  8. washwashed thoroughly with water

Sources & evidence

ORD record
ord-b1c751435ff54ea888fe464c8808333d
Source dataset
uspto-grants-1995_04
Patent number
US05405857

Reaction notes

Loading…