Hydrazine → HCID 178424852, compound

HRID 746706Notes

Reaction equation

HRID 746706 reaction equation
O=[C:2]([CH2:6][C:7]1[C:12]([CH3:13])=[CH:11][C:10]([CH3:14])=[CH:9][C:8]=1[CH3:15])[CH2:3][C:4]#[N:5].[NH2:16][NH2:17]>CCO>[CH3:15][C:8]1[CH:9]=[C:10]([CH3:14])[CH:11]=[C:12]([CH3:13])[C:7]=1[CH2:6][C:2]1[CH:3]=[C:4]([NH2:5])[NH:16][N:17]=1

Participants

4

Reactant 2

HCID 9321HydrazineHCID 22241648HCID 22241648, compound

Product 1

HCID 178424852HCID 178424852, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

3-Oxo-4-(2,4,6-trimethyl-phenyl)-butyronitrile (1.37 gms.) is then suspended in 20 mL of anhydrous EtOH. This suspension is treated with 0.428 mL of anhydrous hydrazine, and subsequently is heated to refluxing temperature overnight. The reaction mixture is cooled to room temperature and evaporated to dryness in vacuo to yield 1.73 gms. of a yellow oil. This oil is then triturated with warm ethyl acetate for 45 min. to provide a yellow-white precipitate. Collection of this precipitate by filtration provides the desired 5-(2,4,6-trimethyl-benzyl)-2H-pyrazol-3-ylamine in the amount of 0.498 gms.

Workup

  1. temperaturesubsequently is heated
  2. temperatureto refluxing temperature overnight
  3. customevaporated to dryness in vacuo
  4. customto yield 1.73 gms
  5. customThis oil is then triturated with warm ethyl acetate for 45 min.
  6. customto provide a yellow-white precipitate
  7. customCollection of this precipitate
  8. filtrationby filtration

Sources & evidence

ORD record
ord-153b06b5fd774d79918046eccfd4fbcd
Source dataset
uspto-grants-2008_07
Patent number
US07393870B2

Reaction notes

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