Sodium Acetate → HCID 178513824, compound

HRID 514679

Reaction equation

HRID 514679 reaction equation
O.O.Cl.[OH:4][C:5]1[NH:9][CH:8]=[N:7][C:6]=1[C:10]([NH2:12])=[O:11].C([O-])(=O)C.[Na+]>Cl>[OH:4][C:5]1[NH:9][CH:8]=[N:7][C:6]=1[C:10]([NH2:12])=[O:11]

Participants

4

Reactant 2

HCID 517045Sodium AcetateHCID 178479550HCID 178479550, compound

Product 1

HCID 178513824HCID 178513824, compoundYield 95.8%

Reagents, catalysts & solvents 1

HCID 313Hydrochloric AcidSolvent

Conditions

Temperature
45 °C

Procedure

Under the nitrogen atmosphere, 10.0 g of 5-hydroxy-1H-imidazole-4-carboxamide hydrochloric acid salt dihydrate prepared according to the method of Reference Example 2 was added to 120 mL of 0.45 mol/L hydrochloric acid and dissolved therein by heating to 40 to 50° C. At 50° C., 25 mL aqueous solution containing 10.3 g of sodium acetate was added dropwise thereto. pH of the reaction mixture was 4.0. After the dropwise addition was completed, the reaction solution was cooled to room temperature and stirred for 1 hour. The crystal was collected by filtration and then washed with a mixture liquid containing 10 mL of acetone and 20 mL of water followed by 30 mL of acetone to obtain 6.1 g of 5-hydroxy-1H-imidazole-4-carboxamide.3/4 hydrate as a gray crystal. The infrared absorption spectrum (ATR method) corresponds to that of Example 4.

Workup

  1. dissolutiondissolved
  2. additionwas added dropwise
  3. additionAfter the dropwise addition
  4. temperaturethe reaction solution was cooled to room temperature
  5. filtrationThe crystal was collected by filtration
  6. washwashed with a mixture liquid
  7. additioncontaining 10 mL of acetone and 20 mL of water

Sources & evidence

ORD record
ord-45c8c3cf8d3348f38353dac2cdea7886
Source dataset
uspto-grants-2015_08
Patent number
US09108928B2

Linked notes

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