반응 #684939

ord-e17cb4e29a2045389be54ddeb6b732f3

반응 방정식

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

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타reacted for 5 hours at 130° C
  2. 2
    온도The mixture is cooled down
  3. 3
    추출The objective material is extracted
  4. 4
    세척The extracted liquid is washed with water
  5. 5
    기타dried
  6. 6
    기타The crude objective material is prepared
  7. 7
    기타by removing the solvent (i.e., N,N-dimethylformamide)
  8. 8
    기타Further, the crude objective material is purified with a column chromatography

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07897313B2uspto-grants-2011_03