反应 #806228

ord-e750f15685eb4227a37c2a101453df7e

反应条件

温度
170°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度heated
  2. 2
    温度The mixture was cooled to 100° C.
  3. 3
    萃取extracted
  4. 4
    workup.ADDITIONby adding toluene (100 ml)
  5. 5
    浓缩concentrated under reduced pressure
  6. 6
    其他crystallized

实验过程

The resulting 12,12-dimethyl-10,12-dihydroindeno[2,1-b]carbazole (7.8 g), iodobenzene (3.7 ml), sodium bisulfite (0.43 g), a copper powder (0.17 g), 3,5-di(tert-butyl)salicylic acid (0.69 g), potassium carbonate (5.71 g), and dodecylbenzene (10 ml) were added to a nitrogen-substituted reaction vessel, heated, and stirred at 170° C. for 10 hours. The mixture was cooled to 100° C., extracted by adding toluene (100 ml), concentrated under reduced pressure, and crystallized using n-hexane (30 ml) to obtain a pale yellow powder of 12,12-dimethyl-10-phenyl-10,12-dihydroindeno[2,1-b]carbazole (8.73 g; yield 88.3%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09196837B2uspto-grants-2015_11