반응 #304729

ord-5fc58a3dfce642d8ad8d587060914a99

반응 조건

온도
150°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타bubbled with nitrogen or argon gas for at least 30 min
  2. 2
    기타to react with VFc or FcA for about 12 h
  3. 3
    기타During the reaction
  4. 4
    기타the solution was also purged with nitrogen (or argon)
  5. 5
    workup.DISSOLUTIONto eliminate dissolved oxygen
  6. 6
    기타After the reaction
  7. 7
    세척was rinsed with dichloromethane, acetonitrile and methanol
  8. 8
    기타dried under a stream of nitrogen gas

실험 절차

Approximately 10 mmol mesitylene solution of vinylferrocene (VFc) or ferrocenecarboxaldehyde (FcA) was put in a round bottom flask and bubbled with nitrogen or argon gas for at least 30 min. A piece of the H-terminated silicon substrate was then immersed in the solution and allowed to react with VFc or FcA for about 12 h under reflux at about 150° C. in an oil bath. During the reaction, the solution was also purged with nitrogen (or argon) to eliminate dissolved oxygen and to prevent the substrate from being oxidized. After the reaction, the substrate derivatized with VFc or FcA was rinsed with dichloromethane, acetonitrile and methanol, and dried under a stream of nitrogen gas. The derivatization of the H-terminated surface with ferrocene moieties as described in Example 2 is illustrated in FIG. 5.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08197650B2uspto-grants-2012_06