3-Methyl-2,4-pentanedione → HCID 118236600, compound

HRID 628503Notes

Reaction equation

HRID 628503 reaction equation
Cl.[Cl:2][C:3]1[CH:8]=[C:7]([NH:9][NH2:10])[CH:6]=[CH:5][C:4]=1[OH:11].[CH3:12][CH:13]([C:17](=O)[CH3:18])[C:14](=O)[CH3:15]>C(O)C>[Cl:2][C:3]1[CH:8]=[C:7]([N:9]2[C:17]([CH3:18])=[C:13]([CH3:12])[C:14]([CH3:15])=[N:10]2)[CH:6]=[CH:5][C:4]=1[OH:11]

Participants

4

Reactant 2

HCID 699493-Methyl-2,4-pentanedioneHCID 68955545HCID 68955545, compound

Product 1

HCID 118236600HCID 118236600, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A mixture of 2-chloro-4-hydrazinophenol hydrochloride salt 3.0 g, 3-methyl-2,4-pentanedione, ethanol 100 ml was stirred with heating under reflux for twelve hours. The solvent was distilled off and thereto was added ethyl acetate 200 ml, and the resulting mixture was stirred for one hour. The precipitates was filtered and was washed with hexane, and was then dried under reduced pressure to give 2-chloro-4-(3,4,5-trimethyl-pyrazol-1-yl)-phenol 3.3 g.

Workup

  1. temperaturewith heating
  2. temperatureunder reflux for twelve hours
  3. distillationThe solvent was distilled off
  4. additionwas added ethyl acetate 200 ml
  5. stirringthe resulting mixture was stirred for one hour
  6. filtrationThe precipitates was filtered
  7. washwas washed with hexane
  8. customwas then dried under reduced pressure

Sources & evidence

ORD record
ord-3952db8740424660895387564010fdaa
Source dataset
uspto-grants-2016_04
Patent number
US09314023B2

Reaction notes

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