HRID221175

反应详情

EQUATION

反应方程式

HRID 221175 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

Under N2 atmosphere, 0.37 parts of 7-bromo-9,9-dibutyl-9H-fluoren-2-ylamine (31), 0.89 parts of 9,9-dibutyl-2-iodo-9H-fluorene (32), 0.17 parts of potassium hydroxide, 0.11 parts of 1,10-phenanthroline, and 0.03 parts of cuprous chloride were added into 10 parts of toluene, followed by stirring and mixing. Then, the reaction mixture was heated to 120° C. and reacted under reflux for 24 hours. After the reaction was quenched by water, diethyl ether was used for extracting the product, and magnesium sulfate was used for dehydration. After removing the solvent, the residual was purified with column chromatography method by using dichloromethane/hexane co-solvent as an eluent, to obtain a compound (33) of the present example. This compound was in a form of a tangerine solid, and the yield of this compound was 57%.

WORKUP

后处理

  1. additionmixing
  2. customreacted
  3. temperatureunder reflux for 24 hours
  4. customAfter the reaction was quenched by water, diethyl ether
  5. extractionfor extracting the product, and magnesium sulfate
  6. customAfter removing the solvent
  7. customthe residual was purified with column chromatography method