HRID535241

反应详情

EQUATION

反应方程式

HRID 535241 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a 1 L Meyer flask, 3.3 g (8.8 mmol) of 2-[4-(9-anthryl)phenyl]benzoxazole, 50 mL of toluene, and 200 mL of ethyl acetate were placed. Into the solution, 1.6 g (8.8 mmol) of N-bromosuccinimide was added little by little. This solution was stirred under air for 25 hours. After a certain period, the solution was washed with water, a saturated aqueous solution of sodium hydrogen carbonate, and saturated saline, and then, the organic layer was dried with magnesium sulfate. The obtained mixture was gravity filtered, and the filtrate was condensed to give an oily substance. The oily substance was purified by silica gel column chromatography (toluene:hexane=5:1) to give a solid. The solid was recrystallized with toluene/methanol, giving 3.3 g of the target yellow powder in a yield of 82%.

WORKUP

后处理

  1. waitAfter a certain period
  2. washthe solution was washed with water
  3. dry with materiala saturated aqueous solution of sodium hydrogen carbonate, and saturated saline, and then, the organic layer was dried with magnesium sulfate
  4. filtrationfiltered
  5. customcondensed
  6. customto give an oily substance
  7. customThe oily substance was purified by silica gel column chromatography (toluene:hexane=5:1)
  8. customto give a solid
  9. customThe solid was recrystallized with toluene/methanol