反応 #684939

ord-e17cb4e29a2045389be54ddeb6b732f3

反応方程式

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

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他reacted for 5 hours at 130° C
  2. 2
    温度The mixture is cooled down
  3. 3
    抽出The objective material is extracted
  4. 4
    洗浄The extracted liquid is washed with water
  5. 5
    その他dried
  6. 6
    その他The crude objective material is prepared
  7. 7
    その他by removing the solvent (i.e., N,N-dimethylformamide)
  8. 8
    その他Further, the crude objective material is purified with a column chromatography

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07897313B2uspto-grants-2011_03