Reaktion #87899

ord-701f055508c44c7799bed306935e5604

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
NCCO
ethanolamine
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
    workup.ADDITIONwas added
  2. 2
    Temperaturheated
  3. 3
    Temperaturto about reflux temperature for about 2 hours
  4. 4
    TemperaturThe mixture was cooled to about 0° C. to about 10° C.
  5. 5
    FiltrationThe reaction mixture was filtered
  6. 6
    Waschenwashed with water (10 mL)
  7. 7
    Sonstigedried in an oven at about 55° C. to about 60° C. for about 12 hours
  8. 8
    Sonstigeto get purple solid

Vorschrift

To 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) in water (40 mL), ethanolamine (2.5 g) was added and heated to about reflux temperature for about 2 hours. The mixture was cooled to about 0° C. to about 10° C. and stirred for about 1 hour. The reaction mixture was filtered, washed with water (10 mL) and dried in an oven at about 55° C. to about 60° C. for about 12 hours to get purple solid.

Quelle

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