HRID591585

反应详情

EQUATION

反应方程式

HRID 591585 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

Under a nitrogen atmosphere, 10 mmol of 2-(1H-pyrazol-1-yl)-9H-carbazole, 10 mmol of 2-bromo-9-(pyridin-2-yl)-9H-carbazole, 1 mmol of copper(I)iodide, 25 mmol of potassium carbonate, and 2 mmol of L-proline were combined in stirring degassed dimethyl sulfoxide. The mixture was heated to 90° C. for 3 days before being cooled and separated between dichloromethane and water. The water layer was washed twice with dichloromethane and the organics were combined and washed once with brine. The organic fraction was dried with magnesium sulfate and concentrated under reduced pressure and subjected to column chromatography of silica with dichloromethane/ethyl acetate as the eluent. After concentrating under reduced pressure, 2′-(1H-pyrazol-1-yl)-9-(pyridin-2-yl)-9H-2,9′-bicarbazole was isolated in a 60% yield.

WORKUP

后处理

  1. customdegassed dimethyl sulfoxide
  2. temperaturebefore being cooled
  3. customseparated between dichloromethane and water
  4. washThe water layer was washed twice with dichloromethane
  5. washwashed once with brine
  6. dry with materialThe organic fraction was dried with magnesium sulfate
  7. concentrationconcentrated under reduced pressure
  8. concentrationAfter concentrating under reduced pressure