反应 #577202

ord-3dbcf8f58861460ba4b48b8b80601a18

反应方程式

F[B-](F)(F)F.N#[O+]
nitrosonium tetrafluoroborate
Nc1ccc(C=Cc2ccccc2)cc1
4-STYRYLPHENYLAMINE
CCOCC
Ether
F[B-](F)(F)F.N#[N+]c1ccc(C=Cc2ccccc2)cc1
desired compound
F[B-](F)(F)F.N#[N+]c1ccc(C=Cc2ccccc2)cc1
4-Styrylbenzenediazonium Tetrafluoroborate

反应条件

温度
-30°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度to warm to −5° C. over 20 min
  2. 2
    过滤the precipitate was filtered
  3. 3
    其他The title compound was purified
  4. 4
    其他by re-precipitating from acetonitrile (3 mL) with ether (15 mL)

实验过程

To a 25 mL round bottom in a drybox was added nitrosonium tetrafluoroborate (0.11 g, 0.95 mmol). Acetonitrile (2 mL) was added and the flask was cooled down to −30° C. A solution of 4-STYRYLPHENYLAMINE (0.17 g, 0.86 mmol) and BHT (0.19 g, 0.86 mmol) in acetonitrile (5 mL) was added dropwise via syringe. The reaction was allowed to warm to −5° C. over 20 min. Ether (10 mL) was then added and the precipitate was filtered. The title compound was purified by re-precipitating from acetonitrile (3 mL) with ether (15 mL) to yield 0.82 g (34%) of the desired compound.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07527831B2uspto-grants-2009_05