Hydrochloric Acid → HCID 178481777, compound

HRID 1291223Notes

Reaction equation

HRID 1291223 reaction equation
[NH2:1][C:2]1[C:3](=[O:10])[N:4]([CH3:9])[N:5]=[CH:6][C:7]=1[NH2:8].Cl.[N:12]([O-])=O.[Na+]>O>[CH3:9][N:4]1[C:3](=[O:10])[C:2]2[N:1]=[N:12][NH:8][C:7]=2[CH:6]=[N:5]1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 127272614,5-Diamino-2-methylpyridazin-3(2H)-oneHCID 23668193Sodium Nitrite

Product 1

HCID 178481777HCID 178481777, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Procedure

In water (10 ml) was dissolved 4,5-diamino-2-methyl-3(2H)-pyridazinone (280 mg) followed by addition of concentrated hydrochloric acid (0.5 ml) with ice-cooling. Then, sodium nitrite (290 mg)/water (5 ml) was added dropwise at a temperature not exceeding 10° C. and the mixture was stirred at that temperature for 1 hour and then at 100° C. for 1 hour. This reaction mixture was allowed to stand in the refrigerator for 16 hours and the resulting precipitate was collected by filtration, rinsed with water, and dried. White powder, 262 mg. 1H-NMR (DMSO-d6) δ: 3.76(3H,s), 8.71(1H,s).

Workup

  1. temperaturecooling
  2. customexceeding 10° C.
  3. waitat 100° C. for 1 hour
  4. waitto stand in the refrigerator for 16 hours
  5. filtrationthe resulting precipitate was collected by filtration
  6. washrinsed with water
  7. customdried

Sources & evidence

ORD record
ord-97cc51c2622c46bda682c72f44df0dfb
Source dataset
uspto-grants-1998_05
Patent number
US05753664

Reaction notes

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