Sulfuric Acid → HCID 69462687, compound

HRID 1247845Notes

Reaction equation

HRID 1247845 reaction equation
[F:1][CH2:2][CH2:3][N:4]1[C:8]([NH2:9])=[C:7]([N:10]=O)[CH:6]=[N:5]1.[S:12](=[O:16])(=[O:15])([OH:14])[OH:13]>O.CO.[Pd]>[S:12]([OH:16])([OH:15])(=[O:14])=[O:13].[F:1][CH2:2][CH2:3][N:4]1[C:8]([NH2:9])=[C:7]([NH2:10])[CH:6]=[N:5]1

Participants

6

Reactant 2

HCID 1118Sulfuric AcidHCID 21904559HCID 21904559, compound

Product 1

HCID 69462687HCID 69462687, compoundYield 95.2%

Reagents, catalysts & solvents 3

HCID 23938PalladiumCatalystHCID 887MethanolSolventHCID 962WaterSolvent

Procedure

To a solution of 1-(2-fluoroethyl)-4-nitroso-1H-pyrazol-5-amine (4.8 g) in water (30 ml) and methanol (30 ml) were added sulfuric acid (2.98 g) and 10% palladium on carbon (2.5 g), and the mixture was hydrogenated under balloon pressure for 7.5 hours. The reaction mixture was filtered through a bed of Celite, and the filtrate was concentrated in vacuo. 2-Propanol was added to the residue, and the precipitate was collected by filtration to give 1-(2-fluoroethyl)-1H-pyrazole-4,5-diamine sulfate (7 g).

Workup

  1. filtrationThe reaction mixture was filtered through a bed of Celite
  2. concentrationthe filtrate was concentrated in vacuo
  3. addition2-Propanol was added to the residue
  4. filtrationthe precipitate was collected by filtration

Sources & evidence

ORD record
ord-6ee5df7b411a4686ae13db1a89f61bf2
Source dataset
uspto-grants-2006_10
Patent number
US07129232B2

Reaction notes

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