Sulfuric Acid → HCID 135515802, compound

HRID 230102Notes

Reaction equation

HRID 230102 reaction equation
N([O-])=O.[Na+].N[C:6]1[N:11]=[N:10][C:9]([CH3:12])=[C:8]2[N:13]=[CH:14][NH:15][C:7]=12.S(=O)(=O)(O)[OH:17]>O.C(O)(=O)C>[CH3:12][C:9]1[C:8]2[N:13]=[CH:14][NH:15][C:7]=2[C:6](=[O:17])[NH:11][N:10]=1

Participants

6

Reactant 3

HCID 1118Sulfuric AcidHCID 23668193Sodium NitriteHCID 24851119HCID 24851119, compound

Product 1

HCID 135515802HCID 135515802, compound

Reagents, catalysts & solvents 2

HCID 176Acetic AcidSolventHCID 962WaterSolvent3×

Conditions

Temperature
50 °C

Procedure

A solution of 4.00 g sodium nitrite in 15 ml of water is added dropwise at 50° C. to 2.20 g of 4-amino-7-methyl-3H-imidazo[4,5-d]pyridazine in a mixture of 30 ml acetic acid, 5 ml of water and 0.5 ml concentrated sulphuric acid. The reaction mixture is stirred for a further two hours at 50° C. and then heated to 90° C. for one hour. After cooling to ambient temperature the reaction mixture is diluted with 30 ml of water. The precipitate formed is suction filtered, washed with water, ethanol and diethyl ether and dried.

Workup

  1. temperatureheated to 90° C. for one hour
  2. temperatureAfter cooling to ambient temperature the reaction mixture
  3. customThe precipitate formed
  4. filtrationfiltered
  5. washwashed with water, ethanol and diethyl ether
  6. customdried

Sources & evidence

ORD record
ord-e31acb7111444e2580230662885bd7a5
Source dataset
uspto-grants-2009_07
Patent number
US07566707B2

Reaction notes

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