Ammonia → HCID 135674107, compound

HRID 392312Notes

Reaction equation

HRID 392312 reaction equation
[NH3:1].[F:2][C:3]1[N:8]=[C:7]([C:9](=[NH:11])[O-])[C:6](=[O:12])[NH:5][CH:4]=1>C(O)C>[F:2][C:3]1[N:8]=[C:7]([C:9](=[NH:1])[NH2:11])[C:6](=[O:12])[NH:5][CH:4]=1

Participants

4

Reactant 2

HCID 222AmmoniaHCID 135674106HCID 135674106, compound

Product 1

HCID 135674107HCID 135674107, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent2×

Procedure

At an ice-cooled temperature, gaseous ammonia was introduced into 2.0 mL of ethanol to prepare a saturated solution, and then 0.10 g of 6-fluoro-3-oxo-3,4-dihydro-2-pyrazinecarboximidoate and 2.0 mL of ethanol were added. After elevating the temperature to room temperature, the mixture was left to stand for 17 hours. The deposited solid product was collected by filtration and washed with ethanol. The residue thus obtained was purified by silica gel column chromatography [eluent: chloroform:methanol=10:1], ethanol was added to the purified product, and the solid product was collected by filtration. Thus, 20 mg of 6-fluoro-3-oxo-3,4-dihydro-2-pyrazinecarboximidamide was obtained.

Workup

  1. customto prepare a saturated solution
  2. customto room temperature
  3. waitthe mixture was left
  4. filtrationThe deposited solid product was collected by filtration
  5. washwashed with ethanol
  6. customThe residue thus obtained
  7. customwas purified by silica gel column chromatography [eluent: chloroform:methanol=10:1], ethanol
  8. additionwas added to the purified product
  9. filtrationthe solid product was collected by filtration

Sources & evidence

ORD record
ord-f7f4c34748e842308fd923b742864116
Source dataset
uspto-grants-2004_10
Patent number
US06800629B2

Reaction notes

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