HRID266605

反应详情

EQUATION

反应方程式

HRID 266605 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

0.70 g (2.17 mmol) of perylene-3,4-dicarboxylic anhydride is mixed with 0.49 g (3.28 mmol) of 4-t-butylaniline, 3.00 g of imidazole and 0.10 g of zinc acetate dihydrate and the mixture is heated at 140°-150° C. for 5 h. While still hot, the mixture is treated with 100 ml of ethanol, and then 200 ml of 10% hydrochloric acid are added. The red suspension is heated until all the ethanol has evaporated, and the product is then filtered off with suction. The red-brown residue is boiled in 10% potassium carbonate solution, the solid residue is filtered off with suction while hot and rinsed several times with hot dist. water. The red residue is dried in a drying cabinet at 120° C. and then recrystallized by extraction with a toluene/methanol mixture to give 0.80 g (81%) of red N-(4-t-butylphenyl)perylene-3,4-dicarboximide which shows a red solid fluorescence. M.p. >330° C. Rf (CHCl3 /silica gel)=0.35.

WORKUP

后处理

  1. temperaturethe mixture is heated at 140°-150° C. for 5 h
  2. customhas evaporated
  3. filtrationthe product is then filtered off with suction
  4. filtrationthe solid residue is filtered off with suction while hot and
  5. washrinsed several times with hot dist
  6. customThe red residue is dried in a drying cabinet at 120° C.
  7. customrecrystallized by extraction with a toluene/methanol mixture