Hydrochloric Acid → HCID 178489312, compound

HRID 1700549Notes

Reaction equation

HRID 1700549 reaction equation
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[CH:9]1[CH2:17][C:16]2[NH:15][N:14]=[C:13]([CH3:18])[C:12]=2[C:11](=O)[CH2:10]1.[C:20]([NH:23][NH2:24])([NH2:22])=[NH:21].[ClH:25].Cl.O>C(O)C>[ClH:25].[NH:23]([N:24]=[C:11]1[CH2:10][CH:9]([C:4]2[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=2[O:2][CH3:1])[CH2:17][C:16]2[NH:15][N:14]=[C:13]([CH3:18])[C:12]1=2)[C:20]([NH2:22])=[NH:21]

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 178418668HCID 178418668, compoundHCID 178489315HCID 178489315, compound

Product 1

HCID 178489312HCID 178489312, compoundYield 110.2%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A mixture of 6-(2-methoxyphenyl)-3-methyl-4,5,6,7-tetrahydroindazol-4-one (0.2 g), aminoguanidine hydrochloride (0.095 g), concentrated hydrochloric acid (0.12 ml), water (0.12 ml) and ethanol (30 ml) was refluxed for 1 hour. Under reduced pressure, the solvent was evaporated, and to the residue was added water. The mixture was washed with ethyl acetate and concentrated under reduced pressure, and the resulting crystals were recrystallized from water-ethanol to give 4-guanidinoimino-6-(2-methoxyphenyl)-3-methyl-4,5,6,7-tetrahydroindazole hydrochloride (Compound 25) (0.3 g) as colorless crystals.

Workup

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

Sources & evidence

ORD record
ord-920cf8e2711d44689fa7a1919a076b9c
Source dataset
uspto-grants-2002_02
Patent number
US06350749B1

Reaction notes

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