반응 #1833208

ord-90c4f38b5631428ab33260dd940baba8

반응 조건

온도
50°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the reaction mixture was heated
  2. 2
    온도to reflux for 6 hours
  3. 3
    온도The reaction was cooled to room temperature
  4. 4
    기타The organic layer was separated
  5. 5
    추출the aqueous layer was extracted with ethyl acetate (4×25 mL)
  6. 6
    세척The combined organic layer were washed with brine
  7. 7
    건조dried over Na2SO4
  8. 8
    농축concentrated in vacuo

실험 절차

A well-stirred solution of 2′,3′-Dinitro-3,4,4′,5-tetramethoxy-(Z)-stilbene (0.422 g, 1.08 mmol) in a mixture of acetone-water (2:1) was heated to 50° C. Then sodium thiosulfate (1.88 g, 10.81 mmol, 10.0 equiv) was added and the reaction mixture was heated to reflux for 6 hours. The reaction was cooled to room temperature and water was added. The organic layer was separated and the aqueous layer was extracted with ethyl acetate (4×25 mL). The combined organic layer were washed with brine, dried over Na2SO4 and concentrated in vacuo. The mixture was then subjected to preparative TLC to give the 2′,3′-Diamino-3,4,4′,5-tetramethoxy-(Z)-stilbene.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: USRE045720E1uspto-grants-2015_10