HRID1820568

反应详情

EQUATION

反应方程式

HRID 1820568 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
135 °C

PROCEDURE

实验过程

50 ml of glycerol was introduced into a 100 ml-four-neck flask, and then stirred and heated at 130 to 140° C. for 2 hours while bubbling with nitrogen gas. The glycerol was left to cool to 100° C., and then 1.03 g (5.02 mmol) of 1-phenylisoquinoline and 0.50 g (1.02 mmol) of iridium (III) acetylacetonate were added. The reaction mixture was stirred and heated for 7 hours at around 210° C. under a nitrogen gas flow. After being left to cool to room temperature, the reaction product was added to 300 ml of 1N-hydrochloric acid, and the resulting precipitate was filtered and then washed with water. The precipitate was purified using silica gel column chromatography with chloroform used as an eluent, to yield 0.22 g of a red powder of iridium (III) tris(1-phenylisoquinoline) (26.8% yield). FIG. 1 illustrates the crystal structure of the iridium (III) tris(1-phenylisoquinoline) as obtained from single crystal structure analysis. As can be seen from FIG. 1, this crystal had pores with a diameter of about 0.8 nm.

WORKUP

后处理

  1. customwhile bubbling with nitrogen gas
  2. waitThe glycerol was left
  3. temperatureto cool to 100° C.
  4. stirringThe reaction mixture was stirred
  5. temperatureheated for 7 hours at around 210° C. under a nitrogen gas flow
  6. waitAfter being left
  7. temperatureto cool to room temperature
  8. filtrationthe resulting precipitate was filtered
  9. washwashed with water
  10. customThe precipitate was purified