HCID 178470798, compound → HCID 178470784, compound

HRID 606447Notes

Reaction equation

HRID 606447 reaction equation
S[C:2]1[NH:6][N:5]=[C:4]([CH2:7][C:8]([O:10][CH2:11][CH3:12])=[O:9])[N:3]=1>C(O)C.[Ni]>[NH:6]1[CH:2]=[N:3][C:4]([CH2:7][C:8]([O:10][CH2:11][CH3:12])=[O:9])=[N:5]1

Participants

4

Reactant 1

HCID 178470798HCID 178470798, compound

Product 1

HCID 178470784HCID 178470784, compoundYield 54%

Reagents, catalysts & solvents 2

HCID 935NickelCatalystHCID 702EthanolSolvent

Conditions

Temperature
80 °C

Procedure

A suspension of ethyl (5-mercapto-1H-1,2,4-triazol-3-yl)acetate obtained in Reference Example 13 (2.00 g, 10.7 mmol) and Raney-nickel (5.00 g) in ethanol (20 mL) was stirred at 80° C. for 15 hr. The catalyst was filtered off, and the filtrate was concentrated under reduced pressure. To a suspension of the residue in ethyl acetate was added activated carbon, and the mixture was filtered. the filtrate was concentrated under reduced pressure to give the title compound as a pale-green powder (900 mg, 54%).

Workup

  1. filtrationThe catalyst was filtered off
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. additionTo a suspension of the residue in ethyl acetate
  4. additionwas added
  5. filtrationthe mixture was filtered
  6. concentrationthe filtrate was concentrated under reduced pressure

Sources & evidence

ORD record
ord-ec6dbe2a7c114de798dddae17acccc3d
Source dataset
uspto-grants-2011_03
Patent number
US07915267B2

Reaction notes

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