HRID600167

反应详情

EQUATION

反应方程式

HRID 600167 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

A mixed solution of 5 g of 1,6-dibromopyrene, 2.1 g of benzothiazole, 5 g of cesium carbonate, 0.31 g of cuprous iodide, 0.12 g of triphenylphosphine, 57 mg of palladium acetate and 50 ml of dimethylformamide was heated while stirred under nitrogen gas stream at a temperature of 130° C. for 6 hours. The mixed solution was cooled to room temperature, thereafter filtered and washed with 10 ml of dimethylformamide and 100 ml of dichloromethane. The filtrate was washed twice with 50 ml of water, dried by magnesium sulfate and thereafter evaporated. The filtrate was purified by silica gel column chromatography and vacuum dried to thereafter obtain 1.1 g of 6-bromo-1-(benzothiazole-2-yl)pyrene.

WORKUP

后处理

  1. temperatureThe mixed solution was cooled to room temperature
  2. filtrationfiltered
  3. washwashed with 10 ml of dimethylformamide and 100 ml of dichloromethane
  4. washThe filtrate was washed twice with 50 ml of water
  5. dry with materialdried by magnesium sulfate
  6. customevaporated
  7. customThe filtrate was purified by silica gel column chromatography and vacuum
  8. customdried