Calcium Chloride → HCID 69522585, compound

HRID 856656Notes

Reaction equation

HRID 856656 reaction equation
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([S:10][CH2:11][CH2:12][N:13]2[CH:17]=[N:16][N:15]=[CH:14]2)=[CH:6][CH:5]=1)([O-])=O.[Cl-].[Ca+2].[Cl-]>C(O)C>[NH2:1][C:4]1[CH:9]=[CH:8][C:7]([S:10][CH2:11][CH2:12][N:13]2[CH:14]=[N:15][N:16]=[CH:17]2)=[CH:6][CH:5]=1

Participants

4

Reactant 2

HCID 5284359Calcium ChlorideHCID 69522692HCID 69522692, compound

Product 1

HCID 69522585HCID 69522585, compoundYield 89.8%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A mixture of 4-[2-(4-nitrophenylthio)ethyl]-4H-1,2,4-triazole (1.0 g), reduced iron (1.12 g) and calcium chloride (0.22 g) in 15% hydrous ethanol (30 ml) was heated to reflux for 22 hours. The reaction mixture was concentrated under reduced pressure, and the obtained residue was separated and purified by column chromatography (basic silica gel, ethanol:ethyl acetate.: 1:19→1:9), to give 4-[2-(4-aminophenylthio)ethyl]-4H-1,2,4-triazole (0.79 g) as colorless crystals.

Workup

  1. temperaturewas heated
  2. temperatureto reflux for 22 hours
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. customthe obtained residue was separated
  5. custompurified by column chromatography (basic silica gel, ethanol:ethyl acetate.: 1:19→1:9)

Sources & evidence

ORD record
ord-d6ecae97c6fd44919849e3e1232031e9
Source dataset
uspto-grants-2007_08
Patent number
US07262185B2

Reaction notes

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