Реакция #684939

ord-e17cb4e29a2045389be54ddeb6b732f3

Уравнение реакции

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

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеreacted for 5 hours at 130° C
  2. 2
    ТемператураThe mixture is cooled down
  3. 3
    ЭкстракцияThe objective material is extracted
  4. 4
    ПромывкаThe extracted liquid is washed with water
  5. 5
    Другоеdried
  6. 6
    ДругоеThe crude objective material is prepared
  7. 7
    Другоеby removing the solvent (i.e., N,N-dimethylformamide)
  8. 8
    ДругоеFurther, the crude objective material is purified with a column chromatography

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07897313B2uspto-grants-2011_03