Ammonium Acetate → HCID 68677556, compound

HRID 2233016Notes

Reaction equation

HRID 2233016 reaction equation
C([O:3][C:4]([C:6]1[N:10]([CH2:11][C:12](=O)[C:13]([CH3:16])([CH3:15])[CH3:14])[C:9](=[O:18])[N:8]([C:19]([CH3:22])([CH3:21])[CH3:20])[N:7]=1)=O)C.C([O-])(=O)C.[NH4+:27]>CO>[C:19]([N:8]1[C:9](=[O:18])[N:10]2[CH:11]=[C:12]([C:13]([CH3:16])([CH3:15])[CH3:14])[NH:27][C:4](=[O:3])[C:6]2=[N:7]1)([CH3:22])([CH3:21])[CH3:20]

Participants

4

Reactant 2

HCID 517165Ammonium AcetateHCID 68675630HCID 68675630, compound

Product 1

HCID 68677556HCID 68677556, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

A solution of 8.60 g of the product of Step C and 21.30 g of ammonium acetate in MeOH was heated in a sealed system at 100° C. for 24 h. The solution was cooled to ambient temperature and concentrated to leave an oil that was partitioned between EtOAc and water. The aqueous layer was acidified to pH 5 with concentrated HCl and then extracted with EtOAc. The combined organic layers were washed with sat. sodium chloride, dried over sodium sulfate, filtered, and concentrated to provide 2,6-di-tert-butyl-2H,7H-[1,2,4]triazolo[4,3-a]pyrazine-3,8-dione as a white solid. MS (M+H+)=265.3.

Workup

  1. concentrationconcentrated
  2. customto leave an oil that
  3. customwas partitioned between EtOAc and water
  4. extractionextracted with EtOAc
  5. washThe combined organic layers were washed with sat. sodium chloride
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated

Sources & evidence

ORD record
ord-256a1cf901e64a268c09b48ce576c220
Source dataset
uspto-grants-2010_05
Patent number
US07709473B2

Reaction notes

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