HRID1066437

反应详情

EQUATION

反应方程式

HRID 1066437 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
160 °C

PROCEDURE

实验过程

To a 250 mL round-bottomed flask fitted with a magnetic stirrer, a condenser and a nitrogen atmosphere are charged 6.26 g (0.0164 mol) of the product of Example 2, 12.8 g (0.116 mol) of resorcinol, 2,4 g of NAFION® NR50 beads 10-35 and 2 mL of xylene. The mixture is heated to 160° C. for 8.5 hours and then allowed to cool to room temperature. A 2.13 g (0.0160 mol) of aluminum chloride is added all at once. The mixture is then heated to 160° C. for two hours. An aliquot is worked up by adding portions of 2N hydrochloric acid and heptane and collecting the solid by vacuum filtration. 1H nmr (CDCl3) reveals a complete conversion to the title compound.

WORKUP

后处理

  1. customTo a 250 mL round-bottomed flask fitted with a magnetic stirrer, a condenser
  2. temperatureto cool to room temperature
  3. temperatureThe mixture is then heated to 160° C. for two hours
  4. customcollecting the solid
  5. filtrationby vacuum filtration