HRID1022352

反应详情

EQUATION

反应方程式

HRID 1022352 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 80 mL trifluoroacetic acid in a 250 mL round bottom flask was added dibenzofuran (7.06 g, 42 mmol) and stirred vigorously to dissolve the content at room temperature. The solution was then cooled on ice and 1.2 equivalent 70% HNO3 (4.54 g, 50.40 mmol) in 20 mL trifluoroacetic acid was poured into the stirred solution slowly. After stirring for 30 minutes contents from the flask was poured into 150 mL ice-water and stirred for another 15 minutes. Off white color precipitate was then filtered out and finally washed with 2M NaOH and water. Moist material was then recrystallized from 1.5 L boiling ethanol in the form of light yellow color crystal. 7.2 g of product was isolated.

WORKUP

后处理

  1. dissolutionto dissolve the content at room temperature
  2. additionwas poured into the stirred solution slowly
  3. stirringAfter stirring for 30 minutes contents from the flask
  4. stirringstirred for another 15 minutes
  5. filtrationOff white color precipitate was then filtered out
  6. washfinally washed with 2M NaOH and water
  7. customMoist material was then recrystallized from 1.5 L