Calcium Chloride → HCID 69522088, compound

HRID 856626Notes

Reaction equation

HRID 856626 reaction equation
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([S:10][CH2:11][C:12]2[N:16]([CH2:17][CH2:18][CH3:19])[C:15](=[O:20])[NH:14][N:13]=2)=[CH:6][CH:5]=1)([O-])=O.[Cl-].[Ca+2].[Cl-]>C(O)C>[CH2:17]([N:16]1[C:15](=[O:20])[NH:14][N:13]=[C:12]1[CH2:11][S:10][C:7]1[CH:6]=[CH:5][C:4]([NH2:1])=[CH:9][CH:8]=1)[CH2:18][CH3:19]

Participants

4

Reactant 2

HCID 5284359Calcium ChlorideHCID 69522259HCID 69522259, compound

Product 1

HCID 69522088HCID 69522088, compoundYield 89.1%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

1-nitro-4-[(4-propyl-1H-1,2,4-triazole-5-one-3-yl)methylthio]benzene (0.5 g), reduced iron (0.5 g) and calcium chloride (0.1 g) were added to 85% aqueous solution of ethanol (15 ml), and the mixture was refluxed for 2 hours. The reaction solution was filtered with. Celite, and the solvent of the filtrate was distilled off. The residue was purified by basic silica gel column chromatography (elution solvent: ethyl acetate) to give 4-[(4-propyl-1H-1,2,4-triazole-5-one-3-yl)methylthio]aniline (0.4 g) as pale brown crystals.

Workup

  1. temperaturethe mixture was refluxed for 2 hours
  2. filtrationThe reaction solution was filtered with
  3. distillationCelite, and the solvent of the filtrate was distilled off
  4. customThe residue was purified by basic silica gel column chromatography (elution solvent: ethyl acetate)

Sources & evidence

ORD record
ord-1923f393254d476e8758edf483c9d38c
Source dataset
uspto-grants-2007_08
Patent number
US07262185B2

Reaction notes

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