Reaktion #684939

ord-e17cb4e29a2045389be54ddeb6b732f3

Reaktionsgleichung

COc1ccc(C=Cc2ccc(N(c3ccc(C)cc3)c3ccc(C)cc3)cc2)cc1
4-methoxy-4′-(di-p-tolylamino)stilbene
CC[S-].[Na+]
sodium ethanethiolate
O
water
Cl
hydrochloric acid
Cc1ccc(N(c2ccc(C)cc2)c2ccc(C=Cc3ccc(O)cc3)cc2)cc1
4-hydroxy-4′-(di-p-tolylamino)stilbene

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigereacted for 5 hours at 130° C
  2. 2
    TemperaturThe mixture is cooled down
  3. 3
    ExtraktionThe objective material is extracted
  4. 4
    WaschenThe extracted liquid is washed with water
  5. 5
    Sonstigedried
  6. 6
    SonstigeThe crude objective material is prepared
  7. 7
    Sonstigeby removing the solvent (i.e., N,N-dimethylformamide)
  8. 8
    SonstigeFurther, the crude objective material is purified with a column chromatography

Vorschrift

The above-prepared 4-methoxy-4′-(di-p-tolylamino)stilbene and twice equimolar amount of sodium ethanethiolate are dissolved in N,N-dimethylformamide, and reacted for 5 hours at 130° C. The mixture is cooled down, and then poured into water and neutralized with hydrochloric acid. The objective material is extracted therefrom using acetic acid. The extracted liquid is washed with water, and then dried. The crude objective material is prepared by removing the solvent (i.e., N,N-dimethylformamide) therefrom. Further, the crude objective material is purified with a column chromatography using silica gel. Thus, 4-hydroxy-4′-(di-p-tolylamino)stilbene (i.e., objective material) is prepared.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07897313B2uspto-grants-2011_03