Ethyl Acetate → HCID 57927618, compound

HRID 889153Notes

Reaction equation

HRID 889153 reaction equation
[CH3:1][N:2]1[C:6]([C:7]([NH:9][NH2:10])=[O:8])=[CH:5][C:4]([CH3:11])=[N:3]1.CCCCCCC.[C:19](OCC)(=[O:21])C>ClC(OC(Cl)(Cl)Cl)=O>[CH3:1][N:2]1[C:6]([C:7]2[O:8][C:19](=[O:21])[NH:10][N:9]=2)=[CH:5][C:4]([CH3:11])=[N:3]1

Participants

5

Reactant 3

HCID 8857Ethyl AcetateHCID 8900HeptaneHCID 41738911,3-Dimethyl-1H-pyrazole-5-carbohydrazide

Product 1

HCID 57927618HCID 57927618, compound

Reagents, catalysts & solvents 1

HCID 10426DiphosgeneSolvent

Procedure

After suspending 2,5-dimethyl-2H-pyrazole-3-carboxylic acid hydrazide (CAS 89187-40-6) (1.15 g) in ethyl acetate (10 ml), trichloromethyl chloroformate (0.90 ml) was added dropwise while stirring on ice. Upon completion of the dropwise addition, the mixture was heated to reflux overnight. It was then allowed to cool, n-heptane (10 ml) was added to the reaction mixture, and the precipitate was collected by filtration to obtain the title compound (1.58 g).

Workup

  1. additionwas added dropwise
  2. additionUpon completion of the dropwise addition
  3. temperaturethe mixture was heated
  4. temperatureto reflux overnight
  5. temperatureto cool
  6. filtrationthe precipitate was collected by filtration

Sources & evidence

ORD record
ord-beeb2cfefe014811bd7a321613e1702a
Source dataset
uspto-grants-2012_08
Patent number
US08252810B2

Reaction notes

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