HRID418030

反应详情

EQUATION

反应方程式

HRID 418030 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

3.2 g (14 mmol) of triphenylene was dissolved in 60 mL of trim ethyl phosphate. To the suspension was added 2.23 g (14 mmol) of bromine in 10 mL of trim ethyl phosphate at room temperature under N2. The mixture was then heated up to 80° C. The reaction was monitored by HPLC. The reaction was quenched by pouring into ice water, then extracted with dichloromethane and washed with saturated sodium bisulfate solution. After drying with magnesium sulfate, the solvent was evaporated. The crude product was run through a short silica gel plug using dichloromethane. 3.0 g of product was obtained after drying under vacuum. The product contains triphenylene, 1-bromotriphenylene, 2-bromotriphenylene, and a mixture of dibromotriphenylene isomers.

WORKUP

后处理

  1. customThe reaction was quenched
  2. additionby pouring into ice water
  3. extractionextracted with dichloromethane
  4. washwashed with saturated sodium bisulfate solution
  5. dry with materialAfter drying with magnesium sulfate
  6. customthe solvent was evaporated