Methane → HCID 18975430, compound

HRID 2393421Notes

Reaction equation

HRID 2393421 reaction equation
C([NH:4][C:5]1([CH2:22][CH2:23][CH2:24][CH3:25])[C:17]2[N:16]3[CH:18]=[CH:19][N:20]=[C:15]3[C:14](=[O:21])[NH:13][C:12]=2[C:11]2[CH:10]=[CH:9][CH:8]=[CH:7][C:6]1=2)(=O)C.[ClH:26].C>CO>[ClH:26].[NH2:4][C:5]1([CH2:22][CH2:23][CH2:24][CH3:25])[C:17]2[N:16]3[CH:18]=[CH:19][N:20]=[C:15]3[C:14](=[O:21])[NH:13][C:12]=2[C:11]2[CH:10]=[CH:9][CH:8]=[CH:7][C:6]1=2

Participants

5

Reactant 3

HCID 297MethaneHCID 313Hydrochloric AcidHCID 18975460HCID 18975460, compound

Product 1

HCID 18975430HCID 18975430, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

1.3 g of 10-acetamido-10-butyl-5H,10H-imidazo[1,2-a]indeno[1,2-e]pyrazin-4-one are dissolved in 25 ml of boiling 2N hydrochloric acid and the solution is stirred for 1 hours 30 minutes at boiling, cooled and concentrated to dryness under reduced pressure (15 mmHg; 2 kPa) at 60° C. The product obtained is dissolved in 30 ml of methanol and, after addition of decolorizing charcoal, the solution is filtered. The filter is washed with 10 ml of methanol, and the filtrate and washing are combined, 400 ml of acetone are added and the solution is stored for 1 hour at a temperature in the region of 20° C. The insoluble product formed is isolated by filtration, washed twice with 100 ml in total of acetone and dried under reduced pressure (1 mmHg; 0.13 kPa) at 20° C. 0.83 g of 10-amino-10-butyl-5H,10H-imidazo[1,2-a]indeno[1,2-e]-pyrazin-4-one hydrochloride (1.8 mol of acid per mole of base) is thus obtained, decomposing without melting above 250° C. (Analysis, % calculated C: 57.01, H: 5.56, Cl: 17.32, N: 15.64, O: 4.47, % found C: 56.9, H: 5.4, Cl: 17.5, N: 15.7).

Workup

  1. temperaturecooled
  2. concentrationconcentrated to dryness under reduced pressure (15 mmHg; 2 kPa) at 60° C
  3. customThe product obtained
  4. filtrationthe solution is filtered
  5. washThe filter is washed with 10 ml of methanol
  6. washthe filtrate and washing
  7. addition400 ml of acetone are added
  8. waitthe solution is stored for 1 hour at a temperature in the region of 20° C
  9. customThe insoluble product formed
  10. customis isolated by filtration
  11. washwashed twice with 100 ml in total of acetone
  12. customdried under reduced pressure (1 mmHg; 0.13 kPa) at 20° C

Sources & evidence

ORD record
ord-99c79011e98e4097918f185133d84338
Source dataset
uspto-grants-1998_09
Patent number
US05807859

Reaction notes

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