Reaktion #87900

ord-1d1f81c75f5542a484f84a1d24c3c76f

Reaktionsgleichung

CC1=NN(c2ccc(C)c(C)c2)C(=O)C1=NNc1cccc(-c2cccc(C(=O)O)c2)c1O
3′-{N′-[1-(3,4-dimethylphenyl)-3-methyl-5-oxo-1,5-dihydro-pyrazol-4-ylidene]hydrazino}-2′-hydroxybiphenyl-3-carboxylic acid
CC1=NN(c2ccc(C)c(C)c2)C(=O)/C1=N\Nc1cccc(-c2cccc(C(=O)O)c2)c1O.NCCO
Eltrombopag Olamine

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated at about 55° C. to about 60° C. for 2 hours
  2. 2
    TemperaturThe mixture was cooled to about room temperature
  3. 3
    FiltrationIt was filtered
  4. 4
    Waschenwashed with ethanol (10 mL)
  5. 5
    Sonstigedried in an oven at about 55° C. to about 60° C. for about 12 hours
  6. 6
    Sonstigeto get purple solid

Vorschrift

A mixture of 3′-{N′-[1-(3,4-dimethylphenyl)-3-methyl-5-oxo-1,5-dihydro-pyrazol-4-ylidene]hydrazino}-2′-hydroxybiphenyl-3-carboxylic acid (2 g) and ethanolamine (10 mL) was heated at about 55° C. to about 60° C. for 2 hours. The mixture was cooled to about room temperature and stirred for about 1 hour. It was filtered, washed with ethanol (10 mL) and dried in an oven at about 55° C. to about 60° C. for about 12 hours to get purple solid. Yield: 1.7 g; Melting point: 237.3-237.6° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09440927B2uspto-grants-2016_09