HCID 178418866, compound → HCID 178420160, compound

HRID 2104958Notes

Reaction equation

HRID 2104958 reaction equation
[C:1]1([C:7]2[N:11]=[C:10](S)[NH:9][N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1>CCO.[Ni]>[C:1]1([C:7]2[N:11]=[CH:10][NH:9][N:8]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

Participants

4

Reactant 1

HCID 178418866HCID 178418866, compound

Product 1

HCID 178420160HCID 178420160, compoundYield 89.2%

Reagents, catalysts & solvents 2

HCID 935NickelCatalystHCID 702EthanolSolvent

Procedure

3-phenyl-1,2,4-triazole-5-thiol (1.80 g, 10.2 mmol) and Raney Ni (rinsed with EtOH 3×, 3 g) in 30 mL EtOH was refluxed for 1.5 h. The mixture was filtered and concentrated. The crude yellow oil was redissolved in EtOAc and filtered through 1″ SiO2, then concentrated to afford 1.32 g of Intermediate 17.1 as a white crystalline solid.

Workup

  1. filtrationThe mixture was filtered
  2. concentrationconcentrated
  3. dissolutionThe crude yellow oil was redissolved in EtOAc
  4. filtrationfiltered through 1″ SiO2
  5. concentrationconcentrated

Sources & evidence

ORD record
ord-2add41df076943448c8cab3cff40d265
Source dataset
uspto-grants-2009_08
Patent number
US07576098B2

Reaction notes

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