Réaction #684939

ord-e17cb4e29a2045389be54ddeb6b732f3

Équation de réaction

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

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Autrereacted for 5 hours at 130° C
  2. 2
    TempératureThe mixture is cooled down
  3. 3
    ExtractionThe objective material is extracted
  4. 4
    LavageThe extracted liquid is washed with water
  5. 5
    Autredried
  6. 6
    AutreThe crude objective material is prepared
  7. 7
    Autreby removing the solvent (i.e., N,N-dimethylformamide)
  8. 8
    AutreFurther, the crude objective material is purified with a column chromatography

Mode opératoire

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.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US07897313B2uspto-grants-2011_03