Potassium Hydroxide → HCID 59394772, compound

HRID 884612Notes

Reaction equation

HRID 884612 reaction equation
[OH-].[K+].Cl.NO.[CH3:6][N:7]([CH3:23])[C:8]([C:10]1[N:11]([CH3:22])[N:12]=[C:13]([N:15]2C(C)=CC=C2C)[CH:14]=1)=[O:9]>O.C(O)C>[CH3:6][N:7]([CH3:23])[C:8]([C:10]1[N:11]([CH3:22])[N:12]=[C:13]([NH2:15])[CH:14]=1)=[O:9]

Participants

6

Reactant 3

HCID 14797Potassium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 593947615-(2,5-Dimethyl-pyrrol-1-yl)-2-methyl-2H-pyrazole-3-carboxylic acid dimethylamide

Product 1

HCID 59394772HCID 59394772, compound

Reagents, catalysts & solvents 2

HCID 702EthanolSolvent2×HCID 962WaterSolvent

Procedure

A solution of potassium hydroxide (1.1 g, 19.5 mmol) in water (30 mL) and ethanol (30 mL) is added to a slurry of hydroxylamine hydrochloride (2.7 g, 39 mmol) in ethanol (50 mL). 5-(2,5-dimethyl-pyrrol-1-yl)-2-methyl-2H-pyrazole-3-carboxylic acid dimethylamide (1.6 g, 6.5 mmol) is added and the mixture is refluxed for 48 hours. The contents of the flask are then concentrated under reduced pressure and the residue is suspended in DCM. The suspension is heated to reflux and then cooled down to room temperature, filtered and the filtrate is concentrated to give crude product. MS (ESI) m/z 169.3 (M+1).

Workup

  1. temperaturethe mixture is refluxed for 48 hours
  2. concentrationThe contents of the flask are then concentrated under reduced pressure
  3. temperatureThe suspension is heated
  4. temperatureto reflux
  5. filtrationfiltered
  6. concentrationthe filtrate is concentrated
  7. customto give crude product

Sources & evidence

ORD record
ord-98f25528d1d34cc2aa344d408c9093f0
Source dataset
uspto-grants-2012_08
Patent number
US08242125B2

Reaction notes

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