Hydrochloric Acid → HCID 178434187, compound

HRID 1700671Notes

Reaction equation

HRID 1700671 reaction equation
[Cl:1][C:2]1[S:3][C:4]([Cl:18])=[CH:5][C:6]=1[CH:7]1[CH2:15][C:14]2[NH:13][N:12]=[C:11]([CH3:16])[C:10]=2[C:9](=O)[CH2:8]1.Cl.[NH2:20][NH:21][C:22]([NH:24][OH:25])=[NH:23].Cl>C(O)C>[ClH:1].[Cl:1][C:2]1[S:3][C:4]([Cl:18])=[CH:5][C:6]=1[CH:7]1[CH2:15][C:14]2[NH:13][N:12]=[C:11]([CH3:16])[C:10]=2[C:9](=[N:20][NH:21][C:22](=[NH:23])[NH:24][OH:25])[CH2:8]1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 178434193HCID 178434193, compoundHCID 178479533HCID 178479533, compound

Product 1

HCID 178434187HCID 178434187, compoundYield 156.8%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Conditions

Temperature
90 °C

Procedure

To a mixture of 6-(2,5-dichlorothiophen-3-yl)-3-methyl-4,5,6,7-tetrahydroindazol-4-one (0.211 g) and 1-amino-3-hydroxyguanidine hydrochloride (102 mg) were added ethanol (4 ml) and concentrated hydrochloric acid (0.1 ml), and the mixture was stirred at 90° C. for 4 hours. Under reduced pressure, the solvent was evaporated, and to the residue was ethanol (2 ml). Precipitated crystals were filtered, washed with ethanol and dried to give 6-(2,5-dichlorothiophen-3-yl)-4-(1-hydroxyguanidin-3-yl)imino-3-methyl-4,5,6,7-tetrahydroindazole hydrochloride (Compound 128) (0.225 g) as pale yellow crystals.

Workup

  1. customUnder reduced pressure, the solvent was evaporated
  2. customPrecipitated crystals
  3. filtrationwere filtered
  4. washwashed with ethanol
  5. customdried

Sources & evidence

ORD record
ord-e3e2d3144d6a4be79ca470a1404fe6e8
Source dataset
uspto-grants-2002_02
Patent number
US06350749B1

Reaction notes

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