Hydrochloric Acid → HCID 178434178, compound

HRID 1700544Notes

Reaction equation

HRID 1700544 reaction equation
[CH3:1][C:2]1[C:10]2[C:9](=O)[CH2:8][CH:7]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[Cl:18])[CH2:6][C:5]=2[NH:4][N:3]=1.[C:19]([NH:22][NH2:23])([NH2:21])=[NH:20].Cl.Cl.O>C(O)C>[ClH:18].[NH:22]([N:23]=[C:9]1[CH2:8][CH:7]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=2[Cl:18])[CH2:6][C:5]2[NH:4][N:3]=[C:2]([CH3:1])[C:10]1=2)[C:19]([NH2:21])=[NH:20]

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 178418668HCID 178418668, compoundHCID 1784341903-Methyl-6-(2-chlorophenyl)-4,5,6,7-tetrahydroindazol-4-one

Product 1

HCID 178434178HCID 178434178, compoundYield 174.5%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A mixture of 3-methyl-6-(2-chlorophenyl)-4,5,6,7-tetrahydroindazol-4-one (0.22 g), aminoguanidine hydrochloride (0.098 g), concentrated hydrochloric acid (0.084 ml), water (0.084 ml) and ethanol (40 ml) was refluxed for 4 hours. Under reduced pressure, the solvent was evaporated, and to the residue was added water. The mixture was washed with diethylether and concentrated under reduced pressure, and the resulting crystals were recrystallized from water-ethanol to give 4-guanidinoimino-6-(2-chlorophenyl)-3-methyl-4,5,6,7-tetrahydroindazole hydrochloride (Compound 21) (0.26 g) as colorless crystals.

Workup

  1. temperaturewas refluxed for 4 hours
  2. customUnder reduced pressure, the solvent was evaporated
  3. additionto the residue was added water
  4. washThe mixture was washed with diethylether
  5. concentrationconcentrated under reduced pressure
  6. customthe resulting crystals were recrystallized from water-ethanol

Sources & evidence

ORD record
ord-9ea48866a5d144788da4f1e42ed86ddc
Source dataset
uspto-grants-2002_02
Patent number
US06350749B1

Reaction notes

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