Ammonium Acetate → HCID 54429941, compound

HRID 581699Notes

Reaction equation

HRID 581699 reaction equation
[C:1]([NH:8][CH:9]1[CH2:17][C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:10]1=O)([C:3](OCC)=[O:4])=[O:2].C([O-])(=O)C.[NH4+:23]>C(O)(=O)C>[NH:8]1[C:1](=[O:2])[C:3](=[O:4])[NH:23][C:10]2=[C:11]3[C:16]([CH:17]=[C:9]12)=[CH:15][CH:14]=[CH:13][CH2:12]3

Participants

4

Reactant 2

HCID 517165Ammonium AcetateHCID 15282825HCID 15282825, compound

Product 1

HCID 54429941HCID 54429941, compoundYield 76.1%

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Conditions

Temperature
20 °C

Procedure

1.25 g of 2-ethoxalylamino-1-indanone are added rapidly to a solution of 12.5 g of ammonium acetate in 50 ml of acetic acid brought to reflux under nitrogen. After 18 hours of reflux, the reaction medium is cooled to a temperature in the region of 20° C. The precipitate formed is filtered off, washed copiously with water and dried under a partial vacuum (1 mm Hg; 0.13 kPa) at 50° C. 0.77 g of 1,4-dihydro-5H-indeno[1,2-b]pyrazine-2,3-dione are thereby obtained in the form of a green powder, the melting point of which is above 260° C. (analysis C11H8N2O2 ; 1.18 H2O; % calculated C: 66.00; H: 4.03; N: 13.99; % found C: 65.7; H: 3.9; N: 13.9).

Workup

  1. temperatureto reflux under nitrogen
  2. temperatureAfter 18 hours of reflux
  3. customThe precipitate formed
  4. filtrationis filtered off
  5. washwashed copiously with water
  6. customdried under a partial vacuum (1 mm Hg; 0.13 kPa) at 50° C

Sources & evidence

ORD record
ord-5a5486e6969f4240a7b61db507d4d9a3
Source dataset
uspto-grants-1999_07
Patent number
US05922716

Reaction notes

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