Hydrochloric Acid → HCID 178513824, compound

HRID 514688Notes

Reaction equation

HRID 514688 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].Cl.[OH-].[Na+]>>[OH:4][C:5]1[NH:9][CH:8]=[N:7][C:6]=1[C:10]([NH2:12])=[O:11]

Participants

4

Conditions

Temperature
45 °C

Procedure

Under the nitrogen atmosphere, 1.5 g of thus obtained 5-hydroxy-1H-imidazole-4-carboxamide hydrochloric acid salt dihydrate was added to 18 mL of 0.45 mol/L hydrochloric acid and dissolved therein by heating to 40 to 50° C. To the solution, 6 mL of aqueous solution containing 0.63 g of sodium hydroxide was added dropwise over 10 minutes. pH of the reaction mixture was 6.6. 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 1.5 mL of acetone and 3.0 mL of water followed by 4.5 mL of acetone to give 0.52 g of 5-hydroxy-1H-imidazole-4-carboxamide.3/4 hydrate as a blue crystal.

Workup

  1. dissolutiondissolved
  2. additionwas added dropwise over 10 minutes
  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 1.5 mL of acetone and 3.0 mL of water

Sources & evidence

ORD record
ord-4791852fb0444f4db5f23d3539e6b86d
Source dataset
uspto-grants-2015_08
Patent number
US09108928B2

Reaction notes

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