Methane → HCID 178479550, compound

HRID 514687Notes

Reaction equation

HRID 514687 reaction equation
[OH:1][C:2]1[NH:6][CH:5]=[N:4][C:3]=1[C:7]([NH2:9])=[O:8].[ClH:10].C>>[OH2:1].[OH2:1].[ClH:10].[OH:1][C:2]1[NH:6][CH:5]=[N:4][C:3]=1[C:7]([NH2:9])=[O:8]

Participants

4

Reactant 3

HCID 297MethaneHCID 313Hydrochloric Acid2×HCID 178513824HCID 178513824, compound

Product 1

HCID 178479550HCID 178479550, compoundYield 254.1%

Conditions

Temperature
75 °C

Procedure

100 g of 5-hydroxy-1H-imidazole-4-carboxamide prepared with reference to the method described in Example 9 of Patent Document 1 (International Publication No. 2009/035168) was added to 1456 g of 7% hydrochloric acid. After dissolving by heating to 75° C., 4.6 g of activated charcoal (TOKUSEI SHIRASAGI, manufactured by Japan EnviroChemicals, Ltd.) and 14 g of 7% hydrochloric acid were added thereto and stirred for 10 minutes at 75° C. The activated charcoal was removed by filtration and washed with 211 g of 7% hydrochloric acid. The washing liquid was combined with the filtrate. The filtrate was cooled to 20 to 25° C. and stirred for 1 hour. The precipitated crystal was collected by filtration and then washed with 314 mL of 2-propanol twice. By performing the drying under the reduced pressure, 133 g of 5-hydroxy-1H-imidazole-4-carboxamide hydrochloric acid salt dihydrate was obtained as a colorless crystal.

Workup

  1. dissolutionAfter dissolving
  2. customThe activated charcoal was removed by filtration
  3. washwashed with 211 g of 7% hydrochloric acid
  4. temperatureThe filtrate was cooled to 20 to 25° C.
  5. stirringstirred for 1 hour
  6. filtrationThe precipitated crystal was collected by filtration
  7. washwashed with 314 mL of 2-propanol twice

Sources & evidence

ORD record
ord-e2431a54a6f5448b96a668a2bfa83232
Source dataset
uspto-grants-2015_08
Patent number
US09108928B2

Reaction notes

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